Document ypna1dN4zMpO1Bm0aMKrZY103

IN THE UNITED STATES DISTRICT COURT FOR THE DISTRICT OF NEVADA NEVADA POWER COMPANY, A NEVADA CORPORATION, PLAINTIFF, VS MONSANTO COMPANY, A FOREIGN CORPORATION; GENERAL ELECTRIC COMPANY, A FOREIGN CORPORATION; WESTINGHOUSE ELECTRIC CORPORATION, A FOREIGN CORPORATION; AND DOES I XXV, INCLUSIVE, ' DEFENDENTS. CV-S-89-555-LDG-LRL EXHIBITS 19 - 37 TO THE DEPOSITION OF ROBERT EMMET KELLY, M.D. VOLUME I ' TAKEN ON FEBRUARY 15, 1994 MARTIN & ASSOCIATES CERTIFIED COURT REPORTERS 2200 MARKET STREET, SUITE 412 GALVESTON, TEXAS 77550 (409) 762-2222 * FAX (409) 762-8040 WATER PCB-00050886 i NEV 011249 WATER PCB-00050887 TO CHEMICAL COMPANY ' "IT . LOUIS (. t 011312 WATER PCB-00050888 * MONSANTO COMPANY, ST. LOUIS, MISSOURI, U.S.A. =1 fm-- 2 cuo 1*1 m M o(/) o s fl%S33 ^0 I--3 P3" 4/3 4/3 ro fsa 44S0fe '-J o4/5 o4/3 KNCAS-Uyme. II. J. P o _m 1 )o m -j ^6 z m jg a* *3 ff 4S 40 3 i S' o 430 " 3 40 3 5" ! y% o s Oa it & s 'Oo 3Mm. 4330 s S' S3' O 349 3#S$I o o 1? oo = i s' s Z1 Isru o "S 430" fc/l *^m3< 3K 4<3^s So33. C430/t* 084saQ0sr 430 5 =5` s 439 i W3a4S90 4<a=0#s cr NEV 011262 WATER PCB-00050889 810.92 200.08/53 THE PROPER HANDLING OF AROCLORS AND THEIR MIXTURES IN THE ELECTRICAL INDUSTRY Monsanto Chemical Co. JCuMonsanto Organic 800 N. Div. Sales Dept. Lindbergh Blvd. St. Louis 66, Mo. P. C. BENtGNUS RavUaJ January I960 ^ DEPOSITION EXHIBIT <33 NEV 007321 WATER PCB-00050890 INDEX Introduction - Page 1-2 Chapter 1 Page 3-12 Page 3 Page 4 Page 12 Chapter 2 - Page 13-19 Page 13 Page 17 Chapter 3 - Page 20-21A Page 20 Page 21 Chapter 4 - Page 22-25 Page 22 Page 23 Page 25 Chapter 5 - Page 26-28 Page 26 Chapter 6 - Page 29-61 Page 29 Page 31 Page 31 Page 32 Page 38 The Proper Handling Of Aroclorr. And Their Mixtures In The Electrical Industry Procedure For Unloading Tankcars Of Aroclors And Aroclor Mixtures A) Description of the Cars B) Procedure for Unloading the Car C) Drum Packaging Storage Tanks A) Qeneral Description B) Detailed Description Gasketing and Pump Packing (A) Suggested Types Of Packing and Gasketing Materials (B) Gaskets For Askarel Capacitors and Transformers Sampling Methods A The ASTM Standard Method B Monsanto Methods (C) Drum Sampling Laboratory Analysis and Procedure (A) For Treating Aroclors and Their Mixtures with Earth Test Procedures (A) General Information (B) Detailed Instruction and Testing Methods 1. Procedure for Cleaning Electrodes 2. Dielectric Constant and Power Factor 3. Dielectric Strength NV 007322 WATER PCB-00050891 \ Page 44 Page 47 Page 49 Page 51 Page 52 Page 55 Page 59 Chapter 7 - Page 62-73 Page 64 Page 65 Page 66 Page 67 Page 68 Page 69 Page 70 Page 71 Page 72 Page 73 Chapter 8 - Page 74-76 Page 74 Page 74 Page 75 Chapter 9 - Page 77-79 Page 77 Page 77 Page 78 Page 79 4. Resistivity 5. Corrosion and Chemical Stability 6. Inorganic Chlorides 7. Acid Number 8. Moisture 9. Hydrolysis Stability Test for Aroclor 10. Thermal Stability Method for Aroclors Typical Properties Aroclor 1232 Aroclor 1242 Aroclor 1248 Aroclor 125*1 Aroclor 1260 Pyranol 1481 Pyranol 1488 Pyranol 1467 Pyranol 1470 Inerteen PPO Quality Requirements of Aroclors Prior to Use in the Electrical Industry Quality as Supplied to the Electrical Industry Typical Electrical Quality of Aroclors Used in the Industry Capacitor Impregnation Transformer Filling Earth Refinement of Aroclors to Arrive at the Desired Elec trical Qualities Earth Treatment in the Laboratory Preparatory to Analysis Earth Treatment by the Plant ' Manufacturing the Askarel Earth Refinement by the User Capacitor Manufacturers Transformer Manufacturers , The Effeot of Earth Refinement on Removal of Tin Tetraphenyl Scavengers from Transformer Askarel N6V 007323 WATER PCB-00050892 Chapter 10 - Page 80-93 Page 80 Page 83 Contamination Avoidance of Contaminating Askarel Capacitors Avoidance of Contaminating Askarel Transformers Chapter 11 - Page 94-97 Page 94 Page 95 Chapter 12 Page 98-IOO Page 98 Page 99 Page 100 Reworking Contaminated Transformer Askarel Normal Conditions Arced Conditions Dermatology and Toxicology Skin Exposure Exposure to Vapors Vapors from a Severely Arced Askarel Transformer Attachments: Drawing No. 31-20847, The Tank Car Drawing No. 31-20848, Dome Detail Drawing No. 9C-8170-5, The Horizontal Storage Tank Drawing No. D-13362, The Vertical Storage Tank Drawing No 90-8248, The Breather Drawing No 9C-8278, The Varec Gauge Drawing No. 9C-8178, The Unloading Platform NEV 007324 WATER PCB-00050893 THE PROPER HANDLING OF AROCLORS* AND THEIR MIXTURES ' IN THE ELECTRICAL INDUSTRY INTRODUCTION Monsanto's Aroclors*, especially the chlorinated biphenyls including types 12*12, 1248, 1254 and 1260, used alone or in combination with chlorinated benzenes, are commonly used die- /T lcctrlc materials of the askarel class. Askarel is a generic name referring to liquid dielectrics derived from halogenated aromatic hydrocarbons possessing excellent chemical and dielectric stability and firc-reslstance over the temperature ranges and operating conditions required of transformers and capacitors in the electrical industry. The properties of Aroclors and their mixtures, used as dielectrics are described in detail in Chapter 7 entitled, "Typical Properties". These dielectrics are manufactured under very carefully-controlled conditions in order to meet the strict and exacting electrical requirements and properties. The electrical industry's use of these fluids has been largely in accordance with the General Electric Company's patents and developments. *Aroclors - Monsanto's chlorinated biphenyls and chlorinated polyphenyls. Registered U.S. Patent Office. *F. M. Clark, "Electrical Insulation", Chem Engg. News 25. 29V'/ (1947)o -1- NEV 007325 WATER PCB-00050894 Resulting from the wide use of these materials in the industry, trade names have been established to identify them by different manufacturers of electrical equipment. Listed alphabetically the trade names include, "Chlorextol," Allis Chalmers; ''Diaclor,1' Sangamo Electric; "Dykanol," Cornell Dubilier; "Elemex," Line Materials; "Hyvol," Aerovox; "Inerteen," Westlnghouse Electric; "Noflamol," Wagner Electric; and Pyranol," General Electric Company. The purpose of this bulletin is to assist the industry with the proper and safe handling of these dielectric materials in their operations. -2 NV 007326 WATER PCB-00050895 CHAPTER 1 PROCEDURE FOR UNLOADING TANKCARS OF AROCLORS AND AROCLOR MIXTiW-g. : A. Description of the Cars , Aroclor and mixtures of Aroclors with chlorinated benzenes are shipped by Monsanto in two types of insulated tankcars- both of which are either aluminum lined or zinc-tin metallized. One type of car has heating colls inside of the tank and these are in direct contact with the product. The other, a more . widely used type of car, is a double-shell tank with heating colls between the Inner and outer shells. The steam coll connections are at the bottom of the car. Both types of tank- cars are tested for 60 pounds pressure and their steam coils are tested for 200 pounds gauge pressure. The cars are top-unloaded by displacement with dry air containing 10 mg. HrO/cu. ft. maximum. There are two or three connections on the tankcar dome depending on the type of car. Where three connections exist, . one is a two inch diameter unloading line which extends to the ' bottom of the car, the second is a one inch diameter air inlet connection and the third is a two inch diameter pressure safety vent, which Is a thin lead disc adjusted to release any pressure . in .excess of 66 pounds gauge * This safety vent is hooded for protection against dust, dirt or accidental bumping. Where only two connections exist on the dome, one Is the two inch diameter unloading line and the other is the safety vent. On these cars, it is necessary to remove the safety vent and introduce the displacement air through that connection. : .a. NEV 00732? ' WATER PCB-00050896 While the tankcar drawing gives, much detail, we have been asked about the following points not given in the drawing: 1. The distance from the rail track to the top of the dome of the cars is variable. It is 13 feet and 4 inches for the 7)000 gallon cars and ranges from 11 feet to 14 feet for the 8,000 gallon cars. 2. The steam connections are located under the center of the cars.' 3. The steam pipe connection is usually a two inch pipe, but on some cars the pipe size is 1-1/4 inches. 4. American Standard taper pipe threads are used. ** -SA NE 00732a WATER PCB-00050897 Drawing No. 31-20^48 shows in detail the dome of a tankcar with three connections. "A" is the two inch unloading line which`extends to a small sump at the bottom of the car. "B" is the one inch air inlet connection. "C" is the hooded safety vent. The car dome cover with fitted bolts Is shown in the center. It is fitted with an aluminum envelope Qoetze gasket. This drawing also shwa bottom opening in the oar. This can be opened only from the inside of the oar and its purpose la for cleaning operations. It has no use at all in unloading the oar. Drawing No. 31-20847 shows the overall dimensions of the 8,000 gallon Aroclor tankcar. B. Procedure for Unloading the Cars The car should be spotted at an unloading dock similar to the one shown by Drawing No. 9C-8176, The oar must be level and the brakes set properly. "STOP - TANKCAR CONNECTED" signs should be placed fore and aft the car to warn switching crews. * *' * If it is raning or snowing or the humidity Is extremely high, it is not advisable to open the car. In case the car must be sampled and opened during bad weather, a canvas canopy must be placed over the dome of the car. It is preferable to unload the oars under roof or inside the factory. Unless it Is absolutely necessary because of following described situations the dome cover should not be opened until ready for sampling. The dome cover is sealed with a standard railroad wire and eeal, and Monsanto should be notified if this seal is found broken upon receipt of the car. NEV 00 7329 -4- WATER PCB-00050898 The first step in unloading is to inspect the dome and clean around the dome cover to remove all loose dirt, water or snowWiping rags and a brush should be used to clean before the dome cover and connections are opened. Then, the screwed hood over the air-inlet valve should be removed and this valve opened fully and left open while heating the car. A Weston or metal encased thermometer should be inserted through this air-inlet valve opening and the tempera ture of the interior of the car determined. If the car temperature is below the caution temperature shown in the following Table 1, it will be necessary to take the special step of inserting a "hair-pin" heating coll through the dome of the car to preclude rupturing the tankcar seams during the heating period. TABLE I Product ASTM Pour Point C. Temperature C. Below which Caution Must Be Used in Heating Aroclor 1260 Aroclor 1254 Aroclor 1248 Aroolor 1242 Inerteen PPO Pyranol 1467 Pyranol 14J0 Pyranol 1481 + 30 + 40 + 10 -7 + 20 +5 - 19 - 10 Pre-heating is not required'' Pre-heating is not required* Pre-heating is not required* Pre-heating is not required* Except if the material has cooled below -10C. and crystals of scavenger have separated. Then, the material should be heated to 70C. (158P.) yntil complete solution has been accomplished. 5NEV 007330 WATER PCB-00050899 If the dome of the car is to be opened for the pre-heating , v* * operation, it is necessary that it be covered with a clean canvas. Extreme care must be taken to avoid getting dirt or moisture into the car. It is due to the relatively high viscosity of some of the Aroclors at low temperatures that it becomes necessary to form a column of molten material from top to bottom of the car, in the center, to prevent hydraulic pressure build-up which may rupture the tank shell if there is too rapid localized heating when employing the main steam colls. When such pre-heating is required, a satisfactory vent hole can be made by Inserting a "hair-pin1* coil (1/2 inch diameter brass, galvanized, or stainless steel pipe) into the open dome of the car and introducing steam through the coil until there is a column of fluid Aroclor from top to bottom. After the vent hole is melted through the material to the bottom of the car, the "hair-pin" coil should be removed and the dome cover replaced and bolted. Steam is then introduced into the main colls. It is recommended that the steam pressure be limited to 100 pounds gauge pressure, particularly when the coils are in direct contact with the Aroclor. The steam coil outlet should be trapped or throttled with a valve. It will require eight to twenty hours to bring the material to pumping temperature - depending upon weather conditions. It la essential that the air inlet valve be open during the heat ing period in order to vent the tank. c NEV 007331 WATER PCB-00050900 Some calculations have been made to indioate the heat requirements for an Aroclor car. Data for an 8,000 gallon car of Aroclor 1254 ares Specific Gravity = 1.5 Specific Heat = 0.26 Btu/lb./P. Heat requirement for heating Aroclor from 30C. (86P.) to 110C. (230P.) is: 8000 x 1.5 x 8.33 x 0.26 x (230-86) : 3,774,000 Btu. For heating from 30C. (86F.) to only 75C. (l67F.), the heat required is 2,110,000 Btu. A nine horse power boiler operating at 80 psig produces 263 lbs,/hr. of steam with no reused condensate. Returning condensate at 200F. will increase the steam output to 296 lbs./hr. at 80 psig. In the first case, heating to 110C., the over-all heat transfer co-effioient is assumed to be too low to utilize the i00 capaoity of the boiler. A value of 1500 for UA with an average h T of 133P, indicates that the useable steam is 202,000 Btu/hr. or 226 lbs./hr. steam at 80 psig. In the second case the & T is lower and the entire output of the boiler is useable. Tatie II sums up the approximate time calculated to heat Aroclor 1254 in an 8,000 gallon car. NEV 007332 WATER PCB-00050901 TABLE II Nine HP Boiler 100# cap. (no reused condensate) 75# cap. (no reused condensate) Lbs. Steam/Hr. 263 -- 30-110C. -- 18 hrs. (86# cap) 30-756C. 9 hrs. 12 hrs. 100# oap. (condensate @ 200F.) 296 -- 8 hrs. 75# cap. (condensate @ 200P.) -- 18 hrs. 11 hrs. (76# oap) Calculations on a five horse power boiler give heating times of the following order: Five HP Boiler Lbs. Steam/Hr. 30-110C. 30-75C. 100# cap. (no reused condensate) 146 28 hrs. 16 hrs. 100# cap. (condensate <8 200F.) 164 25 hrs. 14 hrs. Aroclor oars can be heated by steam (80-100 psig) to the proper handling temperatures in a reasonable time by using a boiler source capable of producing 200,000 to 300,000 Btu/hr. The times given here are approximate and will act as a guide until experience shows the exact time for this operation. -8NEV 007333 WATER PCB-00050902 1 | The proper handling temperature for the various fluids t is given in the following Table III, which indicates correspondI' i ing viscosity values: i | TABLE III Product Handling and Pumping Temperature C. Approximate Viscosity, S.U.S. no>o f-no* Aroclor 1260 Aroclor 1254 Aroclor 1248 1242 Pyranol 1481 Pyranol 1467 Pyranol 1470 95 - 130 75 - 110 50 - 85 35 - 75 30 - 75 20 - 55* 15 - 45* 100 - 43 100 - 42 100 - 40 100 - 40 100 - 40 100 - 40 100 - 40 Inerteen PPO 20 55 100 - 40 *lf any of the scavenger is out of solution, then the material must be heated at 70 C. (158F.) until it has dissolved. Selection of pumping temperatures for any dielectric not shown on this list or which may be developed in the future should be based on a viscosity of about 100 Saybolt Universal Seconds for average pumping and about 40 S.U.S. for fast pumping. When the material has been heated to pumping temperature, a one-half inch diameter pipe "cross" arrangement containing a pressure gauge, air inlet, pressure relief valve to relieve at 30 Psig, and vent connections, should be connected to the dome air inlet pipe. Then the unloading line should be connected. Rust free and clean galvanized piping or stainless steel pipe should be used for the unloading line. NEV 00731<t WATER PCB-00050903 (At this point a sample is taken as described in Chapter 4,) Dry* air is then introduced into the tankcar and pressure built up to 15 pounds gauge. The two inch valve cock on the stand pipe is opened and the discharge pipe observed to be sure the liquid is being unloaded. To protect the seams in the tankcar, the pressure must not exceed 30 pounds. The car will begin to unload at about 12 pounds pressure. When the oar is empty, the air pressure will drop off rapidly and air will blow out of the vent on the receiving tank. The air flow may be stopped at this point and the tankcar pressure released through the vent valve on the "cross" arrangement After inspecting the car to be sure that it has been completely unloaded, all connections and dome cover should be closed tightly. It is essential that the empty tankcar be sealed immediately after the car is unloaded in order to keep the car filled with dr air during return shipment. *It is essential that the displacement air used for unloading be dried thoroughly by some dehumidfying unit such as soda lime, activated alumina or similar dehydrating agent drying unit. It may be necessary to recharge the dehumidifying unit each time that a ear is unloaded. For unloading a tankcar of Aroclor within three hours, 15 standard cubic feet a minute of air at 15 pounds per square inch gauge pressure and a -100F. dew point should be supplied. If the dry air unit is to be used only for unloading tankcars, a small single tower dryer unit containing a selfcontained reactivating heater is suggested. Two manufacturers of air dryers of this type ares C. M. Kemp Mfg. Co., 405 E. Oliver Street, Baltimore 2, Maryland and Pittsburgh Lectrodryer Corporation, Foot of 32nd Street, Pittsburgh, Pennsylvania. -10- NEV 007335 WATER PCB-00050904 As a final step, it is desired that a standard railroad wire seal be inserted through the slotted bolts of the car fittings. Steam should be released from the car colls and all condensate removed from the colls by blowing with air with the steam trap by-passed. All connections must be replaced as received. Adequate oare should be taken in preparing and sealing the oar for return shipment. . Unloading with dry air as described is the preferred and recommended procedure because it is done with the oar dome closed which avoids contamination. Dry nitrogen may be used instead of dry air. If nitrogen ia used it is essential to notify ua (the supplier) so that we oan'take required safety precautions relative to replacing the nitrogen with air in the returned oar prior to sending our men into it for cleaning. If the oar is unloaded by pumping out of the top, whioh required opening the dome, it is most desirable that the oar be set inside of a building. If this cannot be done, then a canopy or roof should be provided over the oar dome, and the unloading should be done when the weather is dear. A dean centrifugal pump with minimum capacity of 40 gpm. 1b suggested. It will be necessary to prime the pump and only dean askarel should be used to do this. Another method for priming the pump is to use a Penberthy steam Jet, No. 22A available from Penberthy Injector Co., 1242 Holden Ave., Detroit 2, Michigan. (Further pump detail ia given on page 17) - 11 - NEV 007336 WATER PCB-00050905 C. Drum Packaging Drum packaging is made with new and carefully inspected 55-gallon drums. These steel drums are lined with a specially selected baked phenolic coating. An example is NESCO No. 3 lining offered by the National Enameling and Stamping Company, Long Island, New York. Contents of the drums should not be heated by direct application of flame or strip heaters. Radiant heat from steam coils or hot air in a heated room is to be preferred. The screw plug in the drum head is fitted with a metal cap as a safe guard against tampering. The drums should be stored indoors. If outdoor storage cannot be avoided, the drums should be placed in a horizontal position and covered with a tarpaulin. nev 007337 WATER PCB-00050906 CHAPTER 2 STORAGE TANKS A. General Description The storage tanks should be a minimum of 10,000 gallons and preferably 12,000 to 15,000 gallons capacity to accommodate the normal 8,000 gallon tankears. It Is preferable to locate the tanks above ground where they are easily accessible for any changes or repairs. Underground location presents difficulty In this respeot. Especially in cold climates, it is preferable to locate the tanks inside of a building. The tanks should be located conveniently with reference to the tankcar unloading facilities and the area where the dielectric is used. Although Aroclors are non-corrosive to metals, corrosion or rusting of iron and steel equipment (by oxidation) may occur resulting in contamination df the products. The resistance of Aroclors to materials of construction is given in Monsanto Teohnioal Bulletin, OP-115, entitled, "The Aroclors", Page 6. Stainless steel tanks are very satisfactory but relatively expensive. . Stainless steel pipe is relatively difficult to fabricate and it is difficult to make tight leak-proof connec tions . . Storage tanks may be of steel construction if properly metallized with zinc-tin or aluminum on the interior surfaces coming in contact with the Aroclors. -13- NEV 007338 WATER PCB-00050907 The metallizing should be done according to the following procedure? 1. Clean an area of the surface by sand blasting, or a similar method to give a perfectly clean and roughened surface. The area cleaned should not be greater than can be completely metallized within a few hours after cleaning. 2. If zinc-tin metallizing is used, a ooating of zinc 0.005 inches thick should be sprayed on to the cleaned surface. This is followed immediately by a coating of tin 0.007 inches thick. 3. Aluminum metallized surfacing should be about 0.01 inch thick. The detailed procedure for metallizing and cleaning is out lined as follows: a) Sand blast, b) Coat with iron, 0.005 inches thick. (The purpose of this coating is to provide a rougher and better bond for the finish coat of aluminum or the zinc-tin combination.) c) Apply the selected finish coat. d) Fill the tank with tap water and warm it with steam. (If an open steam line is used, do not allow the steam to impinge directly onto the metallized surface of the tank.) e) Drain the tank, f) Fill with cold water and drain, g) Wipe dry and clean with clean diaper cloth or other fabric relatively free of lint, h) Heat the tank to at least 100*0. (212F.) to expell moist air. It would be benefi cial to heat the tank, allow it to cool and pull dry air through it using a dehumidfying breather in the air line, heat again etc., until the tank is full of comparatively dry air. i) Spray about 100 gallons of new, electrical grade Aroclor (not high in viscosity) or electrical grade trichlorobenzene onto the inner walls of the tank, washing the walls thoroughly (avoid breathing any fumes). J) Attach the circulating pump, the lines used, and -14- NEV 007339 WATER PCB-00050908 the filter press fitted with dry paper and circulate the fluid through' the system and the tank. Install new dry filter paper several times in the press during this drying and cleaning operation. Discard the dielectric fluid used for cleaning, k) Partially fill the tank with new Aroclor dielectric and analyze it eleotrically and chemically to determine whether it meets specifications. If all tests are met, then fill the tank with the dielectric. The tanks should be Insulated using, preferably, glass foam beads as supplied by Dow-Corning or Libby-Owens-Pord. The suggested thickness of the glass insulation is one inch minimum to two inches maximum. The glass insulation may be covered with tar material commonly used for weather -proofing. Another type of insulation which may be used instead of the glass is 85# Magnesia-Wool which should be covered also with the weather-proofing tar. The advantage of the glass insul ation is that it is not moisture sensitive as is the case with Magnesia-Wool. If the storage tank is located outdoors, it is best that the insulation be covered with riveted or bolted tin sheeting painted with aluminum p^int. This type of metal surface weathers well and is cleaned easily. All piping must be galvanized and screwed fittings must be back brazed to assure tightness. All handling'pipe lines must be traced with steam lines and insolation applied over the two lines in order to keep the handling lines and the material up to the desired pumping temperature. Usually a one-fourth inch copper steam line running parallel with the handling line will suffice. ' "15" nEv 007340 WATER PCB-00050909 Under very severe conditions of low temperatures, it would be desirable to wind the steam line around the handling line about two turns to the foot. The tanks must be provided with ample pressurized heating coll surface to supply sufficient heat to the material to bring it to the proper temperature for pumping and handling as indicated in Table III. Heating coils should be either metallized steel, or preferably steel coils which have been galvanized after fabrication. It is recommended that the steam pressure on all heating colls should not exceed 100 pounds per square inch gauge; lower pressures may be used where practicable. It is essential that all steam coils be completely free from even minute leaks since this will intro duce water into the product. The steam coils may be introduced as "hair-pin" coils through a manhole at the side and bottom of the tank, or as is most often done. Inserted through the manhole at the top of the tank and then located near the bottom. External heating coils located in the Jacket of the tank may be used but this construction.is more expensive and less efficient than the internal colls. The storage tanks may be fitted with a stirrer, either through the top, side, or bottom of the tank and the propeller blade should be located near the bottom of the tank. However, insertion of a stirrer through the side offers possible source of a leak and since these materials are homogeneous, it is not essential to provide such agitation for the purpose of mixing. ' ^. NEV 0073^1 WATER PCB-00050910 Adequate circulation can also be accomplished by using a centrifugal type pump. Gear pumps or other equipment where wear or chipping of metal parts may introduce contam ination should not be used. The pumps must be of the type designed to handle hot oil. All wetted pump parts should be either stainless steel or bronze. The centrifugal pumps must be provided with a deep stuffing box and proper packing used, as described in Chapter 3. As examples of pumps found completely satisfactory for this service, reference is made to Worthington Worthlte pumps. Blackmer pumps, Dean Bros., Peerless and Dayton Dowd Type C pumps for handling hot oil. Also, a very satisfactory arrangement for mixing or circulating and pumping the fluid from the storage tank is to use a vertical sump pump such as a Taber pump. All storage tanks must be amply provided with a dehumidifying breather such as soda lime, activated alumina, etc., units. ThiB Is essential to prevent moist air from coming in contact with the dielectric. A moisture content above 35 ppm adversely affects the electrical resistivity of these products. Provision should be made to preclude possible leakage of the drier material back into the storage tank and the drier should be inspected periodically to make sure that it is open and not plugged. B. Detailed Description Drawing No. 9C-817O shows the detailed construction of a horizontal 15,000 gallon storage tank for Aroclor and its mixtures which has been found completely satisfactory. ^ 007342 WATER PCB-00050911 The various nozzles on this tank are used as follows, considering them in order from left to right on the drawings 3" nozzle Inlet for recirculation 24" nozzle For future agitator if required (not used) 3" nozzle For soda lime or calcium chloride breather connection. 36 " manhole For inspection, etc. The float guage is located in the center of this manhole. 3" nozzle 24" nozzle Not used. For future agitator if required (not used) . 3" nozzle Not used. 3" nozzle Filling inlet connection. 18" x 26" Oval nozzle For sump pump 3" nozzle For thermometer well (see detail) The two 24" nozzles were originally installed for installa tion of agitators, if required. However, it has been found unnecessary to use agitators in the storage tanks, and these nozzles could be omitted. It has been'found that circulation of the fluid by the sump pump, and into the nozzle at the opposite end of the tank, for several hours gives satisfactory blending of the tank contents. For pumping the dielectric from the storage tank, a Taber pump Company all bronze 2-1/2" x 2" vertical sump pump with monel shaft has been found to be quite satisfactory for the appli cation. -18- NEV 007343 WATER PCB-00050912 The liquid level gauge used in the storage must be gas-tight. The storage tanks are equipped with Vapor Recovery Systems Co.'s "Vareo", gas-tight, automatic tank gauge as shown by drawing No. 90-8278. The storage tanks should be provided with an operating plat form suitable to the customer's conditions of operation. The dehumidifying units used as breathers on the storage tanks can be constructed as shown by Drawing No. 90-8248. The upper portion of the chamber is charged with anhydrous soda lime or another drying agent. Periodic inspection of the drying agent will show the formation of a cake of damp material on top about 1 to 1-1/2 inches deep. This cake should be removed and fresh material recharged. Any suitable construction similar to that shown on Drawing No. 90-8248 may be used for the breather units. Drawing No. D-13362 shows design detail of a 15,000 gallon vertical storage tank. The vertical type tank would seem especi ally desirable when insufficient space is available to accomodate the horizontal type tank. 19~ NEV 007344 WATER PCB-00050913 CHAPTER 3 GASKETING AND PUMP PACKING Aroclora and their mixtures soften and swell natural rubber and many of the synthetic "rubber" materials. Such material not recommended for use include, Hycar P, Koroseal, Perbunan, Neoprene, etc. These materials are known sources of contamination. SUGGESTED TYPES OF PACKING AND GASKETING MATERIALS INCLUDE: 1. For Welded Flanged Pipe Connectionsi Garlock Packing Co., No. $01 or No. 7021, 1/8 inch asbestos fiber ' sheet. A ring of thin aluminum drawn tightly at the flange connections may be used satisfactorily also. 2. For Pumps: Garlock No. 234, No, 431, and Gheveron No. 7050-C are satisfactory packings. Likewise, Durametallio 's spiral asbestos fiber may be used. Johns-Manvllle and others have comparable packing materials. 3. For Valves: Garlock No. 117 braided packing or its equivalent is suggested. 4. Other Resistant Materials: It is indicated that duPont's Teflon, poly tetrafluoroethylene is not attacked by hot (130C.) Aroclor and is to be recom mended as a gasket material. Dow-Cornlng's Silastic, Silicone 180, is very resistant to Aroclor and is suggested for gasket purposes. 5. In some cases cork impregnated under pressure with Chrysler's Cycloweld 55-9 or Armstrong Cork Co.'s 1162-J and cured at 170C. may be used as a gasket material. These are baked phenolic type coatings, 6. Pipe Thread Compounds 1 When necessary to use pipe thread compounds, the following should be satisfac tory if care is taken to prevent the pipe compound from getting on the inside of the pipe, . (a) Plastic Lead Seal - manufactured by Dura- metallic Corporation ' (b) Ordinary white lead NV 007345 -20- WATER PCB-00050914 Usually It Is not necessary to use pipe thread compounds since all screwed pipe fittings should 'be sealed by back brazing. T. All new lines and fittings should be cleaned thoroughly by steaming (for two hours) and dried with air or heat. GASKETS FOR ASKAREL CAPACITORS AND TRANSFORMERS 1. For small capacitors requiring ring seals on the terminals, properly selected Silastic (silicone) tubing is cut to make the ring gasket. 2. The most effective and trouble free seal for transformer lids or covers Is to weld the cover onto the transformer shell. To remove the welded cover a weld cutting tool or bar is used. 3. Cork - Nitrile rubber composition gaskets are sometimes used to combine the desired flow limiting property of cork with the resiliency of nitrile rubber. Only fine grained cork should be used in making this composition gasket. Special gasket cementing compounds such as GE's No. 1276 or No. 880 are used to coat the gaskets to further seal them against the transformer fluid and to accomplish firm bonding to the metal surface. 4. Nitrile rubber gaskets are also used and require no adhesive to make a liquid-tight seal. Exposure of nitrile rubber gaskets to transformer askarel should be kept at a minimum and the gasket should not be compressed beyond 2/3 of the original thick ness. After long time exposure to transformer askarel fluid or its vapor, nitrile rubber is measurably deteriorated. While gaskets made of silicone or Teflon are not attacked, these materials are relatively expensive for use in large sizes. Accordingly, for the most efficient performance it is suggested that welded covers be used on askarel transformers.5 5. Instruments, such as temperature gauges, etc. may be attached to the transformer using flange con nection to pipe located below the liquid level of the fluid in the transformer. Such flange con nections are usually not large in diameter. Accordingly, it seems practical to use Teflon or Silastic gaskets to make these seals, especially since it is known that askarel can migrate thru cork or composition cork gaskets used under the liquid level. 21~ NEV 007346 WATER PCB-00050915 Another satisfactory approach used is to machine the flange surfaces of this type connection. - Then a Splritalllc gasket made of stainless steel ring with asbestos inter liner for resiliency can be used satisfactorily. 6. Screwed pipe fittings on askarel transformers require thorough cleaning of the threads to remove oil, grease and dirt. Then the threads are coated with a compound such as GE*s No. 880 and then tightened. ' -21A- N6V 007347 WATER PCB-00050916 CHAPTER 4 SAMPLING METHODS 1.) The ASTM Standard Method for sampling electrical insulating oils is described in ASTM Designation: D923-49. This describes glass and metal thiefs for sampling drums, cans, and tankcars. A specially designed thief or bomb for sampling tankcars is described, also. A very good instrument of this type is the stainless-steel Bacon Bomb Thief with which samples of the liquid can be drawn from any level of the tankcar. The ASTM procedure describes sample containers, their cleaning and storage. Under general precautions, the ASTM mentions that, "Samples of the fluid shall not be taken until the oil is at least as warm as the surrounding air, because cold oil may condense enough moisture from a humid atmosphere to affect seriously its insulation properties. (In the case of tankcar lots, on some occasions there may be no choice, as it may be necessary to procure samples from a tankcar when the temperature is not above the surrounding air. On such occasions, the temperatv, of oil and air also the humidity if possible, should be noted in the report of test results.) It is undesirable to do any sampling when the relative humidity of the atmosphere exceeds 75 percent, and samples shall never be taken in the rain". -22- NEV 007348 WATER PCB-00050917 Several electrical manufacturers using Aroclor dielectrics, switch the tankcars directly into the plant building or under roof before sampling and unloading. These precautions in handling are taken to avoid any contamination of the fluids which are manufactured under very strict specifications. For example, the specificatim for ionizable chlorides allows no detectable amount, (less than 0.10 parts per million). Moisture may not exceed 20 to 35 parts per million. TankcarB are cleaned and prepared under close inspection before they are filled. When filled, and analysis shows the material in the car to be satisfactory, the car is then sealed with a standard railroad wire and seal inserted through the slots of the dome fittings. Likewise, after the tankcars have been unloaded in the industry, it is requested that the dome fittings should be sealed with a railroad wire and seal. 2.) Monsanto Methods used for sampling tankcars differ somewhat from the ASTM procedure. The modified techniques are used because of their greater simplicity and they have been entirely satisfactory as employed over many years. A sample is never taken when it is raining or snowing, or when there is any chance of contaminated atmosphere moving in the direction of the car. However, in case of an emergency during inclement weather, a canopy is placed over -23- N&V 0073-.' WATER PCB-00050918 the car dome before sampling. A satisfactory sample bottle is a five pint, round amber glass, packer type container fitted with a 38 millimeter Bakelite screw cap with an aluminum or tin cup liner. Bottles of this description can be purchased from the Northwestern Bottle Company, 3144 North Broadway, St. Louis, Missouri according to their No. A-7253. Only new bottles and caps are used. When a shipment of bottles is received, the bottles are capped immediately and stored in their receiving cartons. Prior to use, the exterior of the bottles is wiped with a clean cloth. The simplest sampling device used is a clean stainless steel or aluminum dipper. However, this is not' a generally preferred device because it permits sampling the car from the near surface, only. The sampling device commonly used consists of a stainless steel tube, seven feet long with one end bent into a hook, to serve as a handle and on the other end there is a stainless steel bucket with a perforated bottom. This bucket Is about 5-1/4 inches inside diameter and 6 inches deep to hold the five pint bottle. This bottle is held firmly by a stainless steel collar made to slide along the shaft of the sampling device. This collar has a clamp attachment for fixing it tightly into place where desired around the neck of the bottle. When a car is to be sampled, a new sample bottle is clamped firmly in the bucket. "2^" NE V 007350 WATER PCB-00050919 All dirt Is brushed and wiped away from the car dome area using a clean rag. The car dome is opened and the cap is then removed from the sample bottle. The sampling device is inserted into the car so that the neck of the bottle is at least twelve to eighteen inches below the surface of the fluid. The sample taken is dis carded as its purpose is to rinse the bottle. A portion of the sample is used to rinse the interior of the bottle cap. This procedure is repeated until a minimum of three rinses has been made; each time the sample taken is not put back into the car. These rinses should be discarded. Then the sample is taken and the cap of the bottle is screwed down tightly. When the sample has been obtained, the car dome is replaced. immediately. The exterior of the sample bottle is wiped with a clean cloth and when returned to the laboratory it is further cleaned with a cloth dampened with pure trichlorobenzene. if the sample is to be shipped, the cap is taped with Scotch Tape. The sampling device is also cleaned with pure trichloro benzene and is stored in a dust free, air conditioned room. \3.) Drum Samplings glass thief, thoroughly cleaned with pure trichlorobenzene and dried is used to sample drums. -25- NEV 007351 WATER PCB-00050920 CHAPTER 5 . LABORATORY ANALYSIS AND PROCEDURE FOR TREATING AROCLORS AND THEIR MIXTURES WITH EARTH A sample of the Aroclor or Aroclor mixture taken from the tankcar, or drums, as described In Chapter 4, is analyzed in the laboratory to determine Its quality in accordance with the property values given in Chapter 7. For capacitor use, usually the important properties tested are resistivity, power factor, chlorides, and moisture. For transformer use dielectric strength, resistivity, moisture and chlorides are the important properties. If the sample is out of line with the shipping specifica tions, it is indicated that the sample has become contaminated. In this case, another sample is to be taken and the properties redetermined. If still out of specifications, the sample should be given treatment with earth. Treatment of the dielectric with conditioned Attapulgus earth will bring the electrical properties to the maximum attainable values. While there is complete agreement on the benefits derived from treating with conditioned earth, there is difference of opinion on details of the method, arising from factors such as the following. No doubt, there are differences in the absorbent power of various types of diatomaceous earth with respect to removing moisture, impurities and additives such as stabilizers or scavengers from the dielectric -26- NEW 007352 WATER PCB-00050921 materials. The size of the earth particles, temperature and conditions of activation of the earth, the concentrations used and the temperature, the degree of agitation and time interval at which the dielectric is given earth treatment are all possible variables which are still being studied in various laboratories. The method used by Monsanto for treating the fluid with activated earth in the laboratory is: The absorbent is minus 200 mesh Attapulgus* earth acti vated Just prior to use by heating in shallow trays for four hours at 400C. (752'F.) or for at least twelve hours at 250C. (482F.). At least one quart of the dielectric sample is placed into a clean two liter Pyrex beaker or three necked flask. The beaker or flask should be cleaned Just prior to use in a manner similar to the procedure described in Chapter 6, Method No. 11,751, "Procedure for Cleaning of Electrodes, G.E. Cell and Accessories". The flask or beaker is fitted with a glass or stainless steel agitator.' Heat is applied using either a hot plate or a Olae-Gol mantle and is controlled by a thermostat such as a Fenwal thermo switch with a stainless steel sheath. About 0.1 to 0.2$6 of the activated earth, based on the weight of the liquid is added. *Attapulgus Division, Minerals & Chemicals Corp. of America, 210 West Washington Square, Philadelphia 5> Pennsylvania _07_ NEV 007353 WATER PCB-00050922 The more viscous dielectrics such as Aboclors 1248 and 1254 are heated at about 70* to 80*C. (158 - 176*F.) and the less viscous materials such as Aroclor 1242 and Pyranols 1481, 14671 and 1470 are heated at about 50 to 6o*c. (122 to l40F.). After heating and stirring the sample for about four hours, it is filtered using a clean Pyrex glass suction flask and a Buchner funnel fitted with a Whatman No. 1 or No. 3 filter paper. This apparatus and the bottle into which the treated sample of dielectric is transferred should have been cleaned in a manner similar to the cleaning procedure des cribed in Chapter 6. The earth treated and Mup-graded" sample is then ready for final analysis of its electrical properties. -28- NEV 007354 WATER PCB-00050923 CHAPTER 6 TEST PROCEDURES A. General Information The Monsanto test methods described here with the special equipment used are some of the control tests employed to maintain the quality of Arodors for dielectric use. They are suggested as a guide for test work needed to indicate the quality of the dielectrics used in the manufacture of electrical goods. The most significant electrical tests made on Arodors for capacitors are: 1. Dielectric constant. 2. Power Factor. - 3. Resistivity. For transformer use the most significant electrical tests of Aroclor mixtures are: 1. Dielectric Strength 2. Resistivity. Other than electrical tests, significant .measurements of quality include, moisture, chlorides, thermal and chemical stability. The following terms are defined % Dielectric Constant: The dielectric constant (sometimes called specific inductive capacity) of any substance is equal to the ratio of the capa citance of a condenser when that substance is used as the dielectri to the capacitance when there is a'vacuum between the conductors (for all practical purposes air at ordinary pressures may be used instead of a vacuum). -29- NEW 007355 WATER PCB-00050924 Dielectric Strength: Dielectric strength Is the rupturing strength of an insulating material when subjected to voltage stress under specific conditions and expressed in kilovolts. Breakdown varies with the shape of the electrodes and does not increase directly in proportion to the thickness of the dieleotric. Power Factor: The power factor of a dielectric is the ratio of the energy loss in the dielectric to the "apparent power" in the dielectric. Resistivity: Resistivity is electrical resistance offered to the passage of a steady current. The volume resistivity in ohms-centimeter of an oil is the ratio of the d-c potential gradient in volts per centimeter paralleling the current flow within the sample, to the current density in amperes per square centimeter at a given instant of time and under prescribed conditions, Volume resistivity is expressed in ohm-cm. ^ The analytical procedures described in detail include: 1. METHOD NO. 11,751, "PROCEDURE FOR CLEANING OF ELECTRODES, G.E. CELL AND ACCESSORIES." 2. METHOD NO. 11,608, "DIELECTRIC CONSTANT AND POWER FACTOR." 3. METHOD NO. 11,605, "DIELECTRIC STRENGTH." 4. METHOD NO. 11,607, "RESISTIVITY." 5. METHOD NO. 10,126, "CORROSION AND CHEMICAL STABILITY." 6. METHOD NO. 10,118, "INORGANIC CHLORIDES." 7. METHOD NO. 10,087, "ACID NUMBER." 8. METHOD (MODIFIED) NO. 10,620, "MOISTURE (WATER)." NEV 007356 WATER PCB-00050925 9. Hydrolysis Stability Test. 10.' Thermal Stability Test. Detailed Instruction and Testing Methods. 1. METHOD NO. 11,751, "PROCEDURE FOR CLEANING OF ELEC TRODES, O.E. " Cell and Accessories. a. The Electrode Cleaning Procedure; . 1) Place the electrodes in hot electrical grade Trichlorobenzene for ten minutes. 2) Wash with unheated TCB. 3) Rinse twice with methanol and twice with tap water. 4) Place the electrodes in hot 10# Tri Sodium Phosphate solution. Soak and heat for ten minutes. 5) Wash thoroughly with tap water. CAUTION: After step 5 -- DO NOT TOUCH THE ELECTRODES WITH HANDS! ' 6) Wash with distilled water twice. 7) Dry In drying oven for at least two hours at 120C. b. The Q.E. Cell Cleaning: 1) Reclean the cell before use, when more than 8 hours have elapsed since the previous cleaning. 2) Follow the procedure for the electrodes starting at Step 4. o. Cleaning of the Accessories: 1) Apply the same cleaning procedure as given for the electrodes (Steps 1 to 7) to prepare the glass spacer and beaker for next test. 2) Clean the thermometer in the same manner as the electrodes, except for Step 7* ` 3) Place the wet thermometer (after Step 6) directly in position in the temperature Heating Unit (Modified Fisher Isotemp Oven) and allow to dry. -31- NEV 007357 WATER PCB-00050926 2. METHOD NO. 11,608. "DIELECTRIC CONSTANT AND POWER FACTOR." I. -Apparatus - A. Oscilloscope; Heathklt Model 0-6. B. Constant Temperature Heating Unit; Fisher Isotemp oven. Model 13-245A, modified to include Inter wall connectors. C. A. C. Generators General Radio Type 1302-A D. Amplifier and Null Detector; General Radio type 1231-B with type 1261-A power supply. E. Capacitance Bridges General Radio Co. Capacitance Bridge type 716-C. F. Test cells: G. E. type, concentric cylinder electrodes Catalog #1,559,663. (G.E., Pittsfield, Mass. Transformer Lab.) G. Glass B driver transformer: This is used for 60 cycle measurements to excite the bridge directly from the domestic power line. It has 50 volts output with a 4800 ohm resistor in service. H. Tuned Circuit Filters: General Radio Type 1231-P2 (400 and 1000 cycle) and 1231-P3 (60 cycle). These filters aid in obtaining a more accurate frequency for the measurements by removing harmonics, noise, hum, etc. ' II. Adjustment of Controls on Electrical Appartus A. On Panel No. 1 (Top Panel, Amplifier and Null Detector) a. Turn the 4-way (main power) switch on the upper right hand side to the #3 position to determine the Dielectric Constant at 1000 cycles. Turn this switch to the #2 position for measurementa~aFT>0 cycles. b. Allow the equipment to warm up 10 minutes. c. Turn "GAIN CONTROL" to 6. d. Depress "INPUT 0.03V." button. B. On Panel No. 2 (Oscilloscope) a. Turn "INTEN." to about the 12 o'clock position. CAUTION: Do not allow a high intensity spot to remain stationary on the screen for any length of time. -32- NEV 007358 WATER PCB-00050927 II i b. Using "HOR. POSITION" and "VERT. POSITION" controls center the image on the screen. . i c. Adjust "FOCUS" for sharp line. ! d. Turn "FREQ. SELECTOR" to LOOKC. i e. Turn "FREQ. VERNIER" to 80. ' ! f. Turn "VERTICAL GAIN" to 5. g. Turn "VERTICAL INPUT" to "10 VOLT MAX.". 1 h. Turn "HORIZONTAL GAIN" to about 20. i. Turn "SYNCHORONIZING" to + 20. i J. Turn "SYN." to "EXT. SYN." i k. Turn "GEN." to "SWEEP GEN." i C. On Panel No. 3 (Capacitance Bridge) i * a. Turn "RANGE SELECTOR" switch to "100 C" f for 60 cycle measurements and to "1 KC" for 1000 cycle measurements. i I b. Turn "METHOD SWITCH" to direct. 111 c. Turn "DISSIPATION FACTOR" selector switch to "C>". D. On Panel No. 4 (oscillator) a. Disregard this panel for measurements at 60 cycles. b. On 1000 cycle measurements, depress the No. 10 "MULTIPLY BY" button. c. Set "FREQUENCY DIAL" to 100. d. Turn "OUTPUT" dial so that pointer is at the end of the arrow. e. Depress the "UNBAL. 5000 OHMS" button. When all of the above adjustments are made, the electrical apparatus is ready for measurement of Dielectric Constant and Power Factor. -33- NEV 007359 WATER PCB-00050928 III. Determination of Constants for the Apparatus 1. Carefully assemble the cell which has been cleaned - and dried within the last 8 hours. Refer to Method No. 11,751 for the procedure to use In'clean'lng tHe cells. 2. Place the cell assembly in the Fisher oven which has been adjusted to 25C. 3. Connect the back wire inside the oven to the lead on the inner cylinder of the cell and the front wire to the lead on the outer cylinder of the cell. 4. Connect the cable from the capacitance bridge to the terminals on top of the oven so that the inner wire of the cable goes to the back terminal and the outside mesh casing of the cable (the ground) goes to the front terminal. 5. Remove the thermometer from the top of the oven before going on with the test, fiTls~T8Tmporiant. 6. Make all adjustments on the electrical apparatus as directed in Paitfc I of this method. ' 7. Balance the bridge by rotating the "CAPACITANCE" and "DISSIPATION FACTOR" dials on Panel No. 3 until the wide vertical band on the oscilllscope is adjusted to a minimum width. 8. Record the sum of the readings on the "CAPACITANCE" dial and vernier and call this value A. 9. Remove the beaker containing the cell from the oven and fill it with C.P. benzene to a level 0.737 inches (ca. 3/4 inch) above the top of the concentric cylin ders of the cell. 10. Adjust the temperature of the benzene to 25C. while stirring with a thermometer. 11. Replace the cell in the oven (at 25C.) and make the same electrical connections as in Steps 3 and 4. DO NOT interchange connections, 12. Balance the bridge again as in Step 7 13. Record the sum of the readings on the "CAPACITANCE" dial and vernier and call this value B. 14. Calculate the cell constant by the following equation: Cell Constant, K - B - A (this Is usually 2.27 - 1.0 around 70 mmfd.) -34- NEV 007360 WATER PCB-00050929 15* Remove the cell from the oven and balance the . bridge as In Step 7 with the "CAPACITANCE" and "DISSIPATION" "FACTOR" dials. 16. Record the sum of the readings on the "CAPACITANCE" dial and vernier and call this value F. (capacitance of connecting cable.) " 17. Calculate the CELL LEAD CAPACITANCE by the following equation. WHERE? CELL LEAD CAPACITANCE, Q - A - F - K (this is " usually around 3 mmfd.) A = CAPACITANCE OF ENTIRE SYSTEM IN AIR (SYSTEM CONSTANT) Q - CAPACITANCE OF THE CELL LEADS (CELL LEAD CONSTANT) F 8 CAPACITANCE OF CABLE AND WIRES WHICH CONNECT THE CELL AND CELL LEADS TO THE BRIDGE. (CONNECTOR CONSTANT) K = CAPACITANCE OF THE CELL ALONE (THE CELL CONSTANT) Tabulate the system Constant (A), the Cell Lead Constant (0), the Connector Constant (F), and the Cell Constant (K) on a piece of stiff paper and post them near the instru ment where they can be easily referred to for comparison and calculations. These constants must be checked at least once every three months and in all cases where the Dielectric Constant and/or Power Factor are out of specification. Measurement of Dielectric Constant and Power Factor on ArocIor87~fyr5noIFr~Inerteens, and Trl^etracHloro^ ' benzene blends. ' A. Test Run on Cell to Determine whether It 1b Clean and properly~^ITgnegT~~ ! ' ... .. 1. Carefully assemble a cell which has been cleaned and dried within the past 8 hours. NOTE; Refer to method No. 11,751 for procedure to use in cleaning cells. -35- IMEV 007361 WATER PCB-00050930 2. Adjust the oven control to hold at a temperature - of 100C. for all materials except Trl-Tetra Blends. If a Trl-Tetra blend Is to be tested, adjust the oven to hold a temperature of 25C. 3. Place the empty cell assembly In the oven and connect the back wire Inside the oven to the lead on the Inner cylinder of the cell, and connect the other (front) wire to the lead on the outer cylinder. h. Connect the cables from the capacitance bridge to the terminals on top of the oven so that the inner wire of the cable goes to the back terminal an3 the outside metal casing (ground)goes to the front terminal. 5. Allow 15 minutes for the cell to reach temperature equilibrium inside the oven. 6. Remove the thermometer from the top of the oven eTore~TaRTng"any measurements on tHe bridged ' This is important. 7. Make all the adjustments on the electrical apparatus as directed in Part I of this method, 8. Balance the bridge by rotating the "CAPACITANCE" and "DISSIPATION FACTOR" dials on Panel No. 3 until the wide vertical band on the oscilloscope screen is adjusted to a minimum width. 9. Record the sum of the readings on the "CAPACITANCE" dial and vernier and compare this value with the SYSTEM CONSTANT determined in Part II of this method. IMPORTANT: If the value obtained in Step 9 does not agree with the System Constant A (Part II) within 5 uuf, the cell must be re-cleaned, re-dried, re-assembled, and the test run for the System Constant must be repeated. NOTE: Although the above test run must be made prior to each analysis, the value obtained in Step 9 is not to be used in calculations but is to be used only as a check on the cleanliness and alignment of the cell, -36- NEV 007362 WATER PCB-00050931 Procedure for Testing Materials 10. Remove the cell from the oven and fill the beaker with the material to be tested to a level 0.737 inches (ca 3/4 inch) above the cylinders of the cell. 11. Adjust the temperature of the sample to 100*0. (use hot plate) for all materials except Tri-Tetra blends. For Tri-Tetra blends, adjust the tempera ture of the sample to 25C. using an ice-water bath if necessary. NOTE: Stir sample continuously with a thermometer while adjusting the temperature. 12. Place the cell and sample in the oven and make the same connections from the cell to the bridge as in Steps 3 and 4. DO NOT interchange connec tions . 13. Allow 15 minutes for the cell to reach temperature equilibrium inside the oven. 14. Remove thermometer from the oven before taking a measurement. TKis is ImportanT~ ~. 15. Make the adjustment of controls on the electrical apparatus as directed in Part I of this method. 16. Balance the bridge by rotating the "CAPACITANCE" and "DISSIPATION FACTOR" dials on Panel No. 3 until the wide vertical band on the oscilloscope screen is adjusted to a minimum width. 17. Record the sum of the readings on the "CAPACITANCE" dial and vernier, and call this value X. 18. Record the sum of the readings on the "DISSIPATION FACTOR" dial and switch. Call this value D. Calculations: Dielectric Constant r. . X -F -G --y-- Where: X Capacitance reading from Step 17. F m Connector Constant (Determined in Part II) G Cell Lead Constant (Determined in Part II) K e Cell Constant (Determined in Part 11) -37- NEV 007363 WATER PCB-00050932 power Factor = f x D Where: " f = Test Frequency (60 cycles or 1000 cycles) f0= Frequency of "Range Selector" on Panel No.3 D = Dissipation Factor reading from Step 18. NOTE: When D (dissipation factor) is less than 0.1, the dissipation and power factors differ by less than 0.0005. Therefore, for our measure ments, power factors and dissipation factors are equal. Precision: (Reference: General Radio Manual for Model 716-C Capacitance Bridge) a. Capacitance readings are precise to + 2 mmfd. x mul tiplier reading (+ 0.2$ of full scale for each range) when the dissipation factor is less than 0.01. b. Dissipation Factor (Power Factor) readings are pre cise to + 0.0005 or + 2$ of the dial reading which ever is Targer, for values less than 0.1 for D (Dissipation Factor). 3. METHOD NO. 11,605, "DIELECTRIC STRENGTH." a. Apparatus and General Information The electrical equipment necessary to provide high voltage to permit the determination of dielectric strength of liquid dielectric at commercial power frequencies is basically quite simple. The equipment assembled in the laboratory consists of a high voltage transformer of good design and with a current capacity of 2.43 KVA and with equip ment for control of the voltage and a means of measuring the voltage and to provide safety for the operator. nem 736`' WATER PCB-00050933 It is enclosed in a steel gray crackle finished cabinet measuring 42M high, 22" wide, 17" deep and set on truck casters for easy mobility. Protective equipment incorporated in this apparatus prevents the application of high voltage unless all safeguards are complied with. The door on rear of cabinet must be closed. The cover over the oil must be all the way down and the voltage control must be at 0 position. Failure to comply with these requirements will prevent any action when the red button is depressed. The test cup: Transformers, Voltmeters, and Accessories The askarel testing cup type No. 224809 supplied by General Electric Company is mounted on the top rear of the cabinet. It is protected by a heavy plastic cover, hinged at the rear for accessibility to the receptical. It is equipped with safety contactor so placed that the circuit energizing the high voltage contactor cannot be completed unless the protective cover is completely lowered and in plaoe. It is impossible for the operator or anyone else to touch the testing cup when high voltage is applied. The High Voltage Transformer manufactured by the Kelly-Koett Manufacturing Co. is of the closed core, oil immersed, shell type design. Rate @ 81,000 volt @ 40 millampers. It was recovered from a used X-ray machine purchased quite inexpensively -39- MEV 007365 water PCB-00050934 An auto transformer- from the same X-ray machine is connected so as to limit the out-put voltage of the high voltage secondary to 50,000 volts. The primary of the auto transformer is connected to the secondary of a 2-1/2 KVA powerstat variable auto transformer supplied by the Superior Electric Company. Power to the powerstat is controlled by a 4 con tact 30 amp. solenoid circuit breaker. The voltmeter mounted on top near front edge is connected across the powerstat secondary and is calibrated to read directly in Kilovolts in the range of 0 - 50 K.V. The overload circuit breaker consists of a small relay connected between one side of the high voltage transformer secondary center tap and ground. It is adjusted to break contact on a current drain of about 50 milliampers. The circuit for the coil of the solenoid circuit breaker is wired through the contacts of this relay. -40- NEV 007366 WATER PCB-00050935 t Safety and Operating Controls 1) Door interlock switch located on rear door 2) Test cup cover interlock switch. 3) Powerstat switch mounted on rear of unit arranged so that high voltage contactor cannot be closed unless powerstat is at zero position. 4) Main power switch on front panel. 5) Powerstat voltage control on front panel. 6) High voltage contactor push button on front panel (red). 7) Signal lamps mounted on top around voltmeter. Purpose and operation described in method of use, j b. Procedure 1) Ascertain that the temperature of the material under test is 25 ( 0.5)C. i NOTE: Testing at other temperature is likely to give `variable results which may be misleading. 2) Shake the sample container so as to thoroughly it mix the askarel before filling the test cup. J NOTE: This operation is especially important with used Aroclor as the impurities may settle to the bottom and the test may be misleading. 3) Rinse the testing cup three times with small I portions of the sample to be tested. 4) Immediately after final rinse, fill the cup to a height of not less than 20 mm. (0.787 in.) ii above the top of the electrodes. 5) Rock the cup a few times in order that any entrapped air may escape. Close cover over oil test cup. ti 6) Allow to stand 3 minutes. CAUTION: THIS IS < IMPORTANT. 7. Turn main toggle switch on front panel to "ON" (or up) position. Both green and amber pilot lights on the top at either side of the voltmeter will now glow. NEV 007367 ( -41 WATER PCB-00050936 NOTE: The green signal light Is connected across the 115 volt in-put and denotes that line voltage has ' been applied to operating control circuit. Amber light is connected in series with sensitive switch located under high voltage contactors and connected to its armature. It indicates that high voltage contactor is in its rest position and away from contacts energizing auto transformer. 8) Turn voltage control (large knob on front) to extreme counter-clockwise position. 9) Depress red button on front. This energizes high voltage transformer and circuit breaker and is indicated by amber light going out and the red light directly over voltmeter will light. -- 10) Watch the voltmeter and, while holding the button "IN", turn the voltage control at such speed that will cause voltage as indicated on voltmeter to rise at a rate of 3 K.V. per second. 11) Note and Record the voltmeter reading at break down. 12) Repeat the test until two successive breakdowns occur on each of two fillings of the test cup which do not differ by more than 10$6. Report the average value of these two readings (Step 12) as the Dielectric Strength. If the limit of the instrument is reached before breakdown, report the Dielectric Strength as 50 K.V. at 25C. Cleaning of the test cup: ' . After the test is completed, drain the cup. Flush the cup with benzene. Then fill with Aroclor 1248 and let stand, until the next analysis. -42- NEV 007368 WATER PCB-00050937 NOTEs An exception, when samples of oil from the plant are brought in for test, the cup must be thoroughly cleaned with benzene and carbon tetrachloride before and after running the test The electrodes: ' The testing cup has two electrodes. Both electrodes are movable and have twenty threads to the inch with index notches on both the electrodes and the lock nuts. To set the Gap: Arrange one of the electrodes and the lock nuts with the index marks in line. Move the other elec trode until it comes in firm contact with the first electrode and lock it. Now unsorew the electrode with the index marks in line (Step l) two complete turns and lock it. This will leave a gap of 0.1 inch between faces of the electrodes. Cleaning of the electrodes and the test cup free of carbon coating; The following ASTM method of cleaning shall be followed when it is apparent from visual inspection that the electrode discs of the cup are coated with carbon. Wipe olean with dry calendered tissue paper the electrodes and the test cup. NEV 007369 WATER PCB-00050938 The instrument is equipped with a 115 volt AC power supply which supplies all operating voltages for the bridge indicating circuits and in. addition supplies 500 V DC for application, to the material under test. The instrument is completely enclosed in a waxed finish shielded oak cabinet measuring 8-1/2" wide, 22-1/2" long and 8" high. Approximate weight--26 pounds. Test Electrodes: Two concentric nickel cylinders with feet, obtained from General Electric Company. The inner electrode has outside diameter of 2.8" and a height of 3.25" with area of 184 sq. cm. The outer electrode has an inside diameter of 3" and a height of 3,25" with area of 198 sq. cm. The distance between electrodes is, therefore,,0.1" or 0.254 cm. By theory, electrode constant (K) area/length is 191/0.254 or 752 where average area is 191 sq. cm. Also K - 36 x 10" x C (farads with air as dielectric) or 11.29 x C (mmfd. with air as dielectric). Glass Plate: Pyrex about 3~l/2" diameter with concentric grooves to assist in spacing electrodes. Obtained from General Electric Company. Heating Unit: Assembled in the laboratory and is the same unit -45- NEV 007371 WATER PCB-00050939 described in Dielectric Constant Apparatus (see Method No. 11,608; Equipment). b. Procedure: 1) Assemble the test cell. Place the recently cleaned (within the last 8 hours--see Method No. 11,751j Step 9) electrodes in an 800 ml. beaker, . 2) Measure the capacitance of the test cell (Cg) according to Method No. 11,608 (Dielectric Constant and Power Factor measurements.) 3) Fill the cell assembly until the liquid level is 3/4 inch above the top of the electrodes. 4) Heat the assembly on the hot plate to 100 (+ 0.5)C. 5) Place the assembly inside of the testing oven. 6) Attach top lead (+) on the megohm bridge to inner electrode. 7) Attach other lead to outer electrode. 8) Throw the three switches at the top.of the megohm bridge to "ON" position. 9) Allow 10 minutes for assembly to reach temperature equilibrium inside the oven. DANGER: Make sure control knob is in "CHECK" position. Otherwise, painful shock will result if leads are touched. 10) Bring the galvanometer pointer to zero by turn ing the "ZERO ADJUST" knob in the direction in which the pointer of the galvanometer should move. 11) Turn the control knob to "CHARGE" position for 30 seconds. 12) Turn the control knob to "OPERATE" position and return the galvanometer pointer to zero by ad justment of the "MULTIPLY BY" switch and the megohm dial. 13) Read after 30 seconds. -46- N6V 007372 WATER PCB-00050940 Calculation: Resistivity* - Megohm dial reading (Step 12) x "Multiply By" reading (Step 11) x capacitance of ~ cell (Step 2) in mmfd. x 11.29 x 0.001. Report the result in units of 109 ohm-cm. ^Values of resistivity are qualified by designation of temperature and voltage. These are for this test, 1008C and 500 volts DC. NOTE: It is important that the product under test, electrodes, and beaker be at uniform temperature for this determination. Temperature variations in different parts of the sample will cause the galva nometer zero to change constantly and give misleading results. CAUTION: Inasmuch as measurements must be made at a potential of 500 volts DC a shock hazard exists in the handling of this appartus. With the control knob in the charge and operate position full voltage of the bridge (500 volts) is applied to the positive and low terminals and through the test leads to the electrodes. Do not attempt to handle the electrodes of the test leads unless the control knob is in the "CHECK" position. Possible penalty for failure to observe this precaution -- Painful Shook. 5. METHOD NO. 10,126 "CORROSION AND CHEMICAL STABILITY." a. Apparatus: G.E. Corrosion Apparatus consists of the following: 1) A Corrosion Flask - It is a 300-ml. Pyrex flask -47- NEV 007373 WATER PCB-00050941 with a ground glass 24/40 joint equipped with - a 12-inch straight tube as an air cooled con denser. The air-condenser is painted on the - outside with aluminum. " 2) The Corrosion Apparatus: A transite box 32" long x tf" wide x 5" deep. The top of the box represents a split transite board with 5 holes cut to fit the flasks. The box is heated by two 500-watt, 15 volt G.E. Strip heaters with off-set terminals at one end (23.5" overall length). The heating length of the heating element is covered by a copper strip 19-1/2" long x 4" wide x 1/4" thick. The temperature is controlled by an automatic thermostat with temperature setting indicator. b. Procedures 1) Roll a rectangular (2" x 4") piece of aluminum foil so that it will pass through a ground glass 24/40 Joint of the corrosion test flask. CAUTION: Be careful that after rolling the specimen Hoes~not touch itself at any point. 2) Wash the aluminum foil (Step 1) scrupulously with acetone, distilled water, acetone, benzene, and chloride-free ether. 3) Then place the foil on a clean watch-glass and dry in an oven at 110C. for 30 min. After cleaning handle the specimen with tongs or . Torcepsonly. ^ ^ 4) Weigh accurately on an analytical balance the specimen (Step 3) at room'temperature. 5) Drop the weighed aluminum foil into the chloridefree corrosion flask of the "Q.E. Corrosion Appa ratus ." Rinse out flask with sample and rinse end of condenser with sample. 6) Add 200 ml. of the product under test to the aluminum foil (Step 4 and 5). 7) Set the corrosion flask in the corrosion test appa ratus. -48- NV 007374 WATER PCB-00050942 8) Attach a 12-inch straight-tube air-cooled condenser. - the outside of which is painted with aluminum. ' - 9) Cover the exposed part of the flask with aluminum foil. 10) Heat the flask for 6 (+0.1) hours at 2.10 (+ 5)C. The temperature of the liquid in tie test flask is mea sured indirectly using a thermometer inserted through a cork stopper and into similar liquid contained in an identical flask seated adjacent to the test flask on the heating chamber. 11) At the end of the heating period, detach condenser from the flask before removing it from THenToT~pTatei 12) Remove the flask from the hot plate and cover all of the flask with aluminum foil (when the flask is not on the hot plate.) 13) Without removing the aluminum foil covering of the flask, analyze the product (Step 6) remaining in the corrosion apparatus for? a) Appearance, Color-, and Condition. b) Inorganic (Free) Chlorides-- Apply Method No.10,118 c) Acidity (Acid Number) - Fellow Method No. 10,087 14) With a pair of clean, straight nichrome tongs, remove the aluminum foil specimen (Step 5), wash thoroughly, dry and weigh accurately on an analytical balance in the same manner as before (Steps 2, 3 and 4). Report the corrosion as loss or gain in weight to the nearest O.oOOl g. and the Chemical Stability, as indicated by the analysis of the products "After Corrosion Test", in the same way as reported for the original (as received) material. 6. METHOD NO. 10,118, "INORGANIC CHLORIDES." a. Preparation of Standards: 1) Make a primary standard of 100.0 ppm by weighing 0.1648 g. C.P. Nad into a chloride-free 1 liter volumetric flask. Dilute to the mark and mix thoroughly. Make a 10.0 ppm standard by diluting 100 ml. of the primary standard to 1 liter, and mixing well. For every 0.1 ppm standard, dilute to 10 ml. of the 10 ppm standard to one liter and -49- NEV 007375 WATER PCB-00050943 mix well. A 0.1 ppm beam is considered the very faintest beam perceptible to the eye between 15.45 seconds after adding the AgNOo solution, if the beam intensity is not visible at all, or if easily visible (too strong), discard the solutions and make new standards, 2) Weigh 20.0 g. C.P. AgNOs into a chloride free dark bottle. Add 20 ml? C.P. HNO3 (chloridefree). Dilute to 200 mi, with water. 3) All solutions should be freshly prepared every two weeks and stored in glass-stoppered Pyrex bottles. '* b. Light Sources Employ the 2 battery Perilto flashlight, having a 3-4 mm. light aperture. New batteries must be used frequently in order to perceive beams properly. c. Procedures 1) Thoroughly rinse two separatory funnels with chloride-free water three or four times. Then take an aliquot from each funnel in a test tube which has been rinsed with chloride-free water. Test these aliquots for Tyndall beams by adding 3-5 drops of AgNOa and allowing 45 sec. for full beam to evolve. Absolutely no dust or chloride beam should be present. (Tf beam is present, rinse all equipment with 1:1 HNOo and repeat Step 1). " 2) When funnels are beam-free, drain out all the water except 50 ml. in one and 25 ml. in the other. Heat the water in both funnels tc boiling. (Hold stopper while heating as steam may cause- stopper to fail.) 3) Transfer 50 ml. of the sample from the sample bottle at a temperature of 95-100C. into the separatory funnel containing the 50 ml. of boiling water. (As a precautionary measure, pour some of- the sample from the sample bottle into a waste beaker before adding the 50 ml. to the funnel.) 4) Stopper the funnel and shake vigorously for at least 1 minute, venting frequently through the ' stopcock. (Care must be exercised at all times to touch neither the lower part of the funnel stem nor the ground part of the stopcock.) -50- NEV 007376 WATER PCB-00050944 5) Allow the layers to separate and drain off the sample Into the second funnel containing the 25 ml. of boiling water, (as before, drain off a few ml. of the sample Into a waste beaker before draining the sample Into the second separatory funnel.) It may be necessary to heat the sample when transferring the sample to the second funnel; e.g., Aroclor 12o0. 6) Repeat step 4 and allow the layers to separate. Then drain off the sample Into a waste beaker. 7) Combine both water extracts In one funnel and shake thoroughly. 8) Take approximately a 3.0 ml. aliquot of the water extract out through the bottom of the funnel Into a 3/4" x 6" test tube. Again, first allow a few ml. to drain out before taking the aliquot. (The test tube used should be rinsed with, chloridefree water several times before using.) 9) Add approximately an equal portion of chloridefree ether. (The ether is tested by shaking a portion of it with chloride-free water and testing for Tyndall beam at the end of 45 sec. If beam is present, wash ether several times with chloridefree water until washings show no beam after adding 3-5 drops AgNO^). 10) Shake the ether-water mixture until the emulsion in the sample disappears and the water layer is completely beam free before adding AgNOo. If emulsion is difficult to break, add sample dropwise through the ether and then shake.11 11) Add 3-5 drops of 10$ AgNOj solution and test for chloride beam for 45 sec. exactly. If no beam is present at the end of 45 seconds, report as <0.1 ppm. The very faintest of beams is considered 0.1 ppm. If beam is stronger it will be necessary to compare with standards of 0.15# 0.20 up to 1.0 ppm, adding the 3-5 drops of AgNOo and comparing at the end of 45 sec. The method is precise to the nearest 0.1 ppm. Report results to the nearest 0.1 ppm. METHOD NO. 10,087, "ACID NUMBER." a. Reagents; 1) Nitration grade benzol. -51- oo?3fj> WATER PCB-00050945 2) Anhydrous methanol. 3) A saturated solution of phenol red (phenol sulfonphthaiein) in methanol (approx. 0.1$). 4) A 0.01 N solution of KOK in methanol. b. Procedure*. 1) Place 100 ml. of benzol, 100 ml. of methanol and 0.5 ml. (pipette) of phenol red indicator Into one of two clean dry 500 ml. Erienmeyer flasks. 2) Neutralize carefully with the 0.01 N KOH (to be first definite pink color.) 3) Pour the mixture back and forth between the two flasks several times. If the solution is still neutral, divide it equally between the two flasks, if not, repeat steps 2 and 3. 4) Weigh (+ 0.05 g.) into one of the flasks a 75.0 + 5.0 g. sample and titrate with the 0.01 N, KOH until the sample matches the blank. c. calculations: Acid No. (mg. KOH/gram sample) = ml. 0.01 N KOH x 0.56 . Sample Weight Report the results to the nearest 0.001 if they are below 0.1, otherwise to the nearest 0.01. The method is precise to + 0.002 for acid numbers below 0.01 and to + 0.01 Tn the range of 0.1 to 0.01. NOTE 1: To convert mg. KOH/gram to mg. NaOH/gram, multiply by 0.715. 8. METHOD `MODIFIED NO. 10,620, "MOISTURE (WATER)". ' a. Introductory Comments The Karl Fischer Reagent titration method used in the analytical laboratory involves use of an analyt ical balance to weigh accurately about one drop of water used in preparing the standard. Since .an analytical balance may not be available, the method has been modified and uses a purchased standard water solution as described below. Also, in the laboratory a "Dead Stop" potentiometric method for determining NEV 00737a WATER PCB-00050946 the end point is often used. However, as this equipment may not be available, the procedure ' described below uses the visual indicator change < for determining the end point. bo Apparatus and Reagents: 1) Karl Fischer Burett, Automatic Pyrex No. 5750, l 25 ml. capacity. Ace Glass Company, Vineland, New Jersey. 2) Water Standard in Methanol. No. SO-W-2 {1 ml. ^ 1 mg. H2O) Fisher Scientific Company, 2.800 ( Jefferson Ave., St. Louis, Missouri. 3) Karl Fischer Reagent Solution No. SO-K-2, Fisher Scientific Company. c. Standardization of Karl Fischer Reagent l Into a 500 ml. clean, dry Erlenmeyer flask, place about 100 ml. "Anhydrous" methanol (commercially available, 99*95$). Add Karl Fischer reagent to this blank until the first color change from lemon yellow. It is not necessary to read the burette at this point. Carefully pipette 50 ml. of standard I water solution into the blanked methanol. Refill the Karl Fischer burette. Titrate the solution with gentle swirling to mix, until the same color is obtained as was obtained for the blank. Now read the burette. . ; Moisture value of K.F. reagent in terms of grams HgO per ml. - # (Moisture value of t `(Ml. Standard H2O solution) standard water so } lution in gm. per _____________ ______ ________ml. stated on lab { ml. Karl Fischer Reagent i d. Solvent Mixture: Since the solubility of the different askarels varies, the following solvent mixtures are suggested: !1 Material Anhydrous Benzene Anhydrous Methanol 1 Pyranol 1478 0 ml. 300 ml. Pyranol 1488 100 ml. 200 ml. I Pyranol 1467 100 ml. 200 ml. 1 Pyranol l48l 100 ml. 200 ml. Pyranol 1495 100 ml. 200 ml. I1 All Aroclors 110 ml. 190 ml. Inerteen PPO 100 ml. 200 ml. -53- N6V 007379 WATER PCB-00050947 e. procedure, "Visual End Point." 1) Place 100-300 ml. of dry solvent mixture (c) in a dry 500 ml. ground glass-stoppered Brle.nmeyer flask. 2) Titrate the solvent with K.P. reagent to the visual endpoint, i.e., the first change from the yellow to reddish orange that persists for 30 seconds, Refill the burette. 3) Using a beam balance, weigh to the nearest 0.1 gram by difference, a sample containing 0.03 to 0.06 grams H2O into the flask. 4) Stopper and shake until the sample Is in solution. 5) Titrate the solution with K.P. reagent to the endpoint described in Step 2. Record the volume of K.P. reagent used. Calculation; # HoO a ml. of K.P. reagent x HpO factor x 100 Sample Weight References: Mitchell, J. and Smith, D.M., Chemical Analysis, Vol. 5, Aquametry, Interscience Publishers, Inc., New York, (1948) -54- N6V 007380 WATER PCB-00050948 9- "HYDROLYSIS STABILITY TEST FOR ARC0LOR" Purpose .. To quantitatively determine the presence of unstable chlorine compounds in chlorinated biphenyls (askareis). Principle ' The method is based upon the hydrolysis of unstable chlorine compounds in askarels by methar.oiio sodium hydroxide. The resulting chloride ion is determined potentioineurioaliy by titration with silver r.Iti'ate solution in an essentially nonaqueous medium. The measured chloride ion, reported as parts per million in the askarel sample, is indicative of the relative stability of the askarsl in a dielectric system. Reagents 1. Methanol (chloride free) - 5 liters of methanol are refluxed with 0.5g Analytical Reagent Grade AgNOo for 1/2 hour. The methanol Is then distilled from the AgNCq, discarding the first 100 ml. to flush the apparatus. 90# cf the charge is distilled from the flask and the contents of the flask are discarded. The methanol should be checked to assure purity by titration. The chloride ion concentration should be less than 0.01 ml. of 0.005N AgNC^ per 100 ml. of methanol. 2. Sodium Hydroxide Reagent - Analytical Reagent Grade NaOH (may be obtained from Mallinckrodt Chemical Company) Is used to prepare this reagent. A 0.1N solution is prepared by dissolving 4.0 grams of analytical reagent grade NaOH ir. 1 liter of chloride free methanol. 3. Sulfuric acid - Prepared by a 50 ;50 volumetric dilution of Analytical Reagent Grade concentrated sulfuric acid (can be obtained from Malllr.ckrodt Chemical Company) with chloride free (deionized or distilled) water. The acid is always poured into the water with constant stirring to prevent any dangerous build-up of heat. 4. 0.005N AgNO^ and G.0025N AgNOo - Prepared by dilution of an ampoule of concentrated aqueous AgNOo These ampoules can be obtained from Ariachemica Chemical Limited, Champlain, New York. This reagent may also oe prepared by dissolving 0.8495 g. of Analytical Reagent Grade AgNQ* crystals (may be obtained from Mallinckrodt Chemical Company; in one liter of chloride free water containing 3.0 ml. cf concentrated nitric acid. This solution should be standardized against a pure chloride standard. A sodium chloride crystal such as used in infrared spectrometer cells is a good source of pure NaCl. The AgNOi solutions should be checked (at least monthly) to assure a consistent reagent. -55- NEV 007381 WATER PCB-00050949 5. Acetone (chloride free) - Prepared by distillation from AgNOo as described above, for methanol and should also be checked by potentiometric titration to assure optimum purity. Normally a chloride content of less than 0.01 ml. of 0.0025N AgNOj per 100 ml. is derived by this method. 6. Benzene - Analytical Reagent Grads benzene should be used. This material is normally chloride free but should be checked by potentiometric titration to be certain. Analyti cal Reagent Grade benzene may be obtained from Mallinokrodt Chemical Co. Equipment 1. 200 ml. tall form beaker (Berzelius type). 2. Magnetic stirrer - A suitable magnetic stirrer with ring stand base can be obtained from Fisher Scientific Co. Cat. #14-511-1. This stirrer has a built-in rheostat and should be set at full speed and operated through a variac to adjust its speed. This will prevent heating of the stirrer during the stirring operation. 3. Teflon magnetic stirring bar - The bar should be cylindrical in shape and of one piece molded construction. one inch long, may be obtained from Fisher Scientific Co., Cat. #9-311-9. 4. Microburet graduated in 0.01 ml. divisions - A suitable buret may be obtained from Scientific Glass Apparatus Co., Inc. Bloomfield, New Jersey Cat. #JM-570. 5. Silver electrode - The Beckman silver billet electrode Cat #39261 is the preferred type. 6. Glass electrode - A standard glass electrode such as Beckman electrode Cat. #40498. 7. pH meter suitable for use with glass electrode - A model GS Beckman pH meter can be used. This instrument has the expanded scale and provides greatest sensitivity to incre mental emf changes. A somewhat less sensitive but, nonethe less , useable meter such as Beckman "Zeromatic" or the Leeds Northrop line operated pH meter can be used. 8. Water bath - An individual glass water bath 150mm in diameter 75mm high and containing 600 ml. of water heated to 40C. + 1C. is used. This glass water bath can be obtained from " Corning Glass Co., Corning, N.Y. Cat. #3140. 9. Usual laboratory glassware - 25 ml. pipette, buret or pipette graduated to deliver 0.5 ml., wash bottles for pure acetone methanol, water and a sturdy ringstand. -56- NEV 007382 WATER PCB-00050950 Procedure for 1242 Aroclor (1499 Pyranol) 1. Twenty five grams of askarel is weighed into a tared 200 ml. beaker to the nearest 0.01 gram on a suitable balance. 2. The magnetic stirring bar is then added to the beaker containing the sample (without the bar touching the operators' hands), 3. Twenty five ml. 0.1N NaOH (methanolic) is added by means of a 25 ml. pipette and the beaker is covered with a watch glass. 4. The sample beaker is immersed to a depth of 1 1/4 inches in the 40 4_ 1C. water bath on a magnetic stirrer and clamped securely to a firm support. The sample is stirred at as fast a speed as possible, without pronounced splashing, for 1 hour. The water bath is not heated. No effort is made to maintain the temperature at 4oC., and it will drift toward equilibrium with room temperature. 5. After the 1 hour stir, the sample beaker is removed from the bath, 0.5 ml. of dilute sulfuric acid is added to the sample by means of a suitable pipette or buret. 125 ml. of chloride free acetone Is then added (a graduated cylinder is suitable for this purpose). 6. The sample is then titrated with 0.005N AgNOq solution using the silver-glass electrode system. Normal samples of askarel require extremely small amounts of AgNOo, for this reason the titration is run using 0.01 ml. additions and allowing sufficient time for equilibrium to be established before recording the emf change. If a change of less than Imv per 0.01 ml. addition is observed for 3 or 4 .01 ml. increments, larger additions of AgNOo may be used for instance .05 ml. until such a change isJ observed. The additions then are reduced to 0.01 ml. again to complete the titration. The endpoint normally Is defined by two 50mv changes. A normal titration would yield the illowlng typical data. MV dMV* ML dML dMV/dML r-2 400 0 .06 0 392 8 .07 .01 352 8 . .08 .01 341 11 .09 .01 321 20 .10 .01 271 5.0 .11 .01 221 50 .12 .01 201 20 .13 .01 285 16 .14 .01 0 8 8 11 20 50 50 20 16 Using the GS pH meter the change Is mi units and hence the meter changes observed would be 5 times this value (i.e. 25 units for 5mv). -57- NEV 00 73ti3 WATER PCB-00050951 To calculate the change per 0.01 ml. observed, the mv change Is divided by the volume of AgNOj. By plotting dmv/dml vs. ml., the endpoint may be found to the nearest 0.001-ml. This gives a sensitivity of + O.OOTppm - to define the endpoint to + .01 ml. r.o plotting is necessary and- a sensitivity of + 3.07ppm is assumed. 7. A reagent blank is run exactly as above omitting the askarel sample. Calculations Subtract the reagent blank from the total volume of AgN03 and for the sample then: Reactive Chlorine (ppm) * Net Volume AgN03XNormality AgNO^X35.46xio3 weight : .. Procedure for 1254 and 1260 Aroclors (more viscous askarels) The procedure is followed exactly as above except that under Procedure, Step 2, 5 ml. of benzene is immediately added to the askarel sample and stirring bar. The sample is heated until it dissolves in the benzene and cooled to room temperature before proceeding to Step 3 The benzene, of course, should be Included in the reagent blank determination. Procedure for Micro Test The dechlorination test may also be run on 5 gram samples of askarels with a reduction In sensitivity. It Is run exactly as the 25 gram test above except that the amount of reagents then used are 5-01 ml. NaOH (0.1N methanolic), 0.1 ml. HgSCty for acidification, and 50 ml. of acetone to dilute the sample. 0.0025N AgN03 is used to titrate this size sample. The sensi tivity is then + 0.l8ppm rather than + O.OTppm given by the 25 g sample (without plotting the endpoint). General Comments A rapid titration can be made to the nearest 0.1 ml. using the normal potential at the equivalence point or use can be made of an automatic titrator for routine control procedures. The sensitivity in either case should be within + 0.7ppm of the value obtained by more refined techniques with 0.005N AgN03 and a 25 gram sample. The usual analytical precautions should be exercised in using this test method to prevent cross contamination from other sources of halogen in the laboratory. This means that all glassware, apparatus, and the area in wHXcE~THTs~Test is.run should be ahaTytTcaliy cl'eahT " ---- > :' -58- NEV 00738% WATER PCB-00050952 10. "THERMAL STABILITY METHOD FOR AROCLORS Scope This method measures the thermal stability (chloride content) of chlorinated biphenyls used primarily as dielectrics, it is used for determining the quality of finished Aroclors. Principle Certain impurities if present in chlorinated biphenyls will break down at elevated temperatures with the liberation of HC1. The volatile HC1 is swept out of the sample with air, absorbed in water and titrated with silver nitrate solution. The results are expressed as parts per million chloride obtained during a 16 hour thermal stability test period. Reagents 1. Acetone. No special grade is required. It must contain no titratable chlorides. 2. 1% HNO3. Dilute 1 ml. concentrated HNO3 to 100 ml. 3. 0.005 NAgNOg. 0.8495g to 1000 ml. 5 ml. 0,1 NAgNOg (if available) to 100 ml. Apparatus 1. Pressure Regulator. Moore - Model 40 - 2 - 0-50" Water. Moore Products Co. H & Lycoming St., Philadelphia 24, Pennsylvania. 2. Thermoregulator. Cenco - 99015 - (Central Scientific Co.) 3. Relay. Ebert Micrelay SPST Std. Type. Ebert Electronics Corp., Queens Village, N.Y. (Any sensitive, reliable relay can be used). 4. Stirring Motor. Bodine NSI-13 B-2224 l/40 HP. 1725 R.P.M. 5. Bath Fluid. Dow Corning 550. 5 gallons 6. Leeds & Northrup ac. operated pH Meter - Cat. No. 7664 7. Silver wire electrode . 8. Mercurous Sulfate Reference Electrode. Modified L & N calomel reference electrode prepared as follows. Dismantle the internal element from the salt bridge tube of a standard L & N calomel reference electrode. Discard the saturated KC1 solution from the tube and clean out the mercurous NEV 007365 WATER PCB-00050953 chloride and mercury from the internal element. Clean parts thoroughly. Add sufficient new clean mercury to the internal element to make contact with electrode wire and re-pack chamber of internal element with mercurous sulfate moistened with 0.5M potassium sulfate. Seal the chamber with non-absorbant cotton. Fill the salt bridge tube with 0.5M potassium sulfate and reassemble units. 9. Burette. 1.0 ml. microburette - Koch - Fisher Scientific Co. - 2C-110. 10. Magnetic Stirrer and glass covered stirring bar. 11. Glass Apparatus for Samples in Bath. See attached diagram. 12. capillaries. Glass capillaries approximately 0.2 mm in diameter and cut to a length that permits a flow of 45 ml. per min. of air, 13. Variac. 2 KVA. 14. Air Supply. Air under 4o lb. pressure is available in our laboratories. This air is purified by passing through a scrubber bottle containing 40^ NaOH, an empty bottle which serves as a safety, a second bottle containing cone. H0SO4 and a trap immersed in dry ice and acetone. The purified air is connected to a glass manifold having one connection for each sample. Capillaries of the appropriate length are connected between the manifold and the outlet for each sample. In this manner a constant flow of air can be obtained on all samples by applying a constant pressure to the manifold. 15. Heating Bath. A stainless steel bath constructed according to the specifications given in the attached diagram Is used. The bath is heated by applying 85 Volts to 3-500 Watt G.E. strip heaters bolted to the bottom of the bath. One 500 Watt Immersion heater Is connected to the thermostat. Dow Corning 550 silicone is used as the bath liquid. The tem perature is maintained at 210 + 0.2C. The bath should be placed in hood and the tests carried out In total dark ness. Two 3 X 5" stainless steel plates not shown in the sketch are placed on top of the straightening vanes in the bottom of the bath. This provides better stirring to the ends of the bath. Twelve samples can be run in the bath at one time. . Procedure Weigh a 290 + 1 g. sample of Aroclor into the 300 ml. Erlenmeyer flask. Insert the gas inlet tube and position the flask in the 210 + 0.5C. bath. The bath fluid level should be approximately one inch below the bottom of the ground glass joint on the flask, place 10 ml. distilled water in the Volhard flask absorber and attach to the receiver tube from the Erlenmeyer flask. Connect the purified air supply from the capillary to the inlet down tube ~6" NEV 007386 WATER PCB-00050954 in the flask. Bubble air through the sample for 16 hours at the rate of 35 to 45 ml. per minute. (The apparatus and/or sample must be kept in the dark during the 16 hour period). Transfer the water from the absorber to a 100 ml. beaker using approximately 50 ml. acetone, and 2 drops 1% HNOo solution and titrate with 0.005N AgNO^ solution using a magnetic stirrer. The titration is stopped at 75 mv. which represents the point of maximum potential change and the titration endpoint. Silver wire and. mercurous sulfate electrodes (Ag-Hg, Hg2SC>4, 0.5M K2S04 system) are used for the titration. Calculations (Total ml. 0.005 NAgNOj used) (0.6l) = ppm chloride * 1 ml. 0.005 NAgNOq is equivalent to 0.0001773g. chloride or 0.6l ppm. Precision and Reliability The precision of the test (standard deviation) is 0.02 ppm at the 0.5 ppm chloride level and 0.06 ppm at the 2.8 ppm lev61. The method as written does not necessarily quantitatively measure the total unstable chlorides present. For screening purposes a total chloride figure is not necessary. Experience has shown that there is good correlation between the chloride figures obtained by this 16 hour thermal stability test and the quality of chlorinated biphenyls. Discussion The air supply can be checked for chloride contamination by passing the air through an empty sample flask immersed In the bath. Not more than 0.03 ml. 0.005 NAgNOg should be required to give the endpoint. The air supply can be checked for ammonia by measuring the pK of the absorber solution or titrating with 0.01N HC1. The pH should be between 6 and 7 Compressed cylinder air available for breathing purposes can perhaps be used without any purification. Experience has shown that nitrogen gives low chloride figures. This indicates that air is a neces sary part of this test and that nitrogen cannot be used as a substitute. Gum rubber tubing is used in making all connections. The apparatus is cleaned with acetone. -61- NEV 007387 WATER PCB-00050955 CHAPTER 7 TYPICAL PROPERTIES The 1200 series members of the Aroclor family are chlor inated biphenyls, and are made by chlorinating biphenyl to approximately the percentage of chlorine, by weight, in dicated by the last two digits of the serial number. For example, Aroclor 1254 is approximately 54# chlorine on a weight basis. Accordingly, these Aroclors are not single or simple compounds. They are a mixture of isomeric com pounds composed predominately of the chemical compound in dicated below as being their approximate equivalent: Aroclor 1242 Aroclor 1248 Aroclor 125^ Aroclor 1260 Trichlorobiphenyl Tetrachlorobiphenyl Pentachloroblphenyl Hexachlorobiphenyl . For transformer use and some capacitor- use where lower viscosity is required for better low temperature operation than offered by the above Aroclors, these products are mixed with pour point depressants, particularly trichlorobenzene resulting in various General Electric Company Pyranols described briefly as follows: Transformer Pyranol 1467* 60# of Aroclor 1260 40# of Elec. Grade Trichlorobenzene 0.125# of Tin Tetraphenyl Transformer Pyranol 1470'" 45# of Aroclor 1260 55# of Elec. Grade TrichloroTetrachlorobenzene Mixture 0.125# of Tin Tetraphenyl % "Use of tin tetraphenyl scavenger is subject to G.E. patents and license: Royalty arrangements should be checked before using Pyranol 1467. Questions about license concerning the use of anthraquinone stabilizer for DC capacitors should be referred to Western Electric, 195 Broadway, N.Y.C. -62- 00738a WATER PCB-00050956 Transformer Inerteen PPO 60# of Aroclor 1260 40# of Elec. Grade Trichlorobenzene 0.20# Phenoxypropene oxide Capacitor Pyranol 1481 75# of Aroclor 1254 25# of Elec. Grade Trl- chlorobenzene Detailed properties of all of these products are given in the following property lists. -63- NEV 007389 WATER PCB-00050957 AROCLOR 1232 PROPERTY Vise. 37.8C. (ASTM D88) Specific Gravity @ 25/15.5C. (ASTM D287) Color, APHA Condition ' Clear Acidity, mg. KOH/g. Pcur Point, C. (ASTM D97) Inorganic Chlorides, ppm. Refractive Index 25C. Distillation Range (ASTM D20) Corrected for stem and barometic pressure Corrosion Water Content, ppm Resistivity 100C., 500 volts DC 0.1"gap Dielectric constant 100C. @ 1000 cycles (ASTM D924) Sulfates (ASTM-D117-31)* Fixed Chlorine content (Carius)* Dielectric Strength (KV) (ASTM D877)* Hydrolysis Stability Test Chlorides, ppm. Thermal Stability Test Chlorides, ppm. TYPICAL 44 - 51 1.270 - 1.280 50 Max. 0.014 Max. -30 or lower 0.10 max. 1.6200 - 1.6220 10# - 293C. min. 50# - 310 - 320C. 90# - 360C. max. After heating with aluminum for six hours at 2i0c. i I0c. the aluminum must not be corroded either on visual or weight inspection and the Aroolor 1242 should meet the following specs: Color, APHA 100 max. Acidity, mg.KOH/g. 0.014 max. Inorg. Chlorides, ppm. 0.10 max. Condition dear 35 max. 500 x 10 Ohm-cm., min. 4.3 - 4.5 None 31.5 - 32.5 35 min. 3.0 (tentative) max. 0.5 (tentative) max. *Not determined unless by special request. -64- 00l' WATER PCB-00050958 AROCLOR 1242 PROPERTY - TYPICAL Vise. at-27.8C. (ASTM D88) Specific Gravity at 25/15.pC. (ASTM D287) Color, APHA Condition Acidity, mg. KOH/g. Pour Pt., >C. (ASTM D97) Inorganic Chlorides, ppm. Refractive Index at 25 C. Distillation Range (ASTM D20) Corrected for stem and barometric pressure Corrosion 82 - 92 seconds Saybolt Univer. 1.381 - 1.392 50 max. Clear 0.01 max. -14 or lower No detectable amount 1.6240 - 1.6260 10# 325C. min. 90$ Q60i^fli'. max. After heating with aluminum for six hours at 210C + 10C, the aluminum must not be cor roded either on visual or weight inspection and the Aroclor 1242 should meet the following specs: Water Content, ppm Resistivity 100C. 500 volts DC at 0.1" gap Dielectric Constant 100C. at 1000 cycles (ASTM D924) Flash Point Cleve. Open Cup* Fire Point C. Sulfates (ASTM-D117-31)* Fixed chlorine content (Carlus)* Specific Heat at 25C.* Evaporation at 100C for 6 hrs.* Dielectric Strength (KV) (ASTM D877)* Color, APHA 60 max. Acidity, mg.KOH/g. 0.01 max. Inorg.Chlorides,ppm no detectable ' amount Condition Clear 35 max. 500 x 109 ohm-cm., min. 4.7 - 4.9 170 - 200C. None to boiling point None ' . $43 + 0.50 02 0.4$ max. 35 Min. Not determined unless by special request. Hydrolysis Stability Test chlorides, ppm Thermal Stability Test chlorides, ppm 1.0 (tentative) max. 0.40 (tentative) max. -65- NEV 007391 WATER PCB-00050959 AROCLOR 1248 PROPERTY Vise, at 54.4C. (ASTM D-88) Spec. Gravity at 05/15.5c. (ASTM D-287) Color, APHA Condition Acidity, mg. KOH/g. Pour Point C. (ASTM D-97) Refrac. Index at 20C. Dist. Range (ASTM D-20) Water Content, ppm. Resist. 100C. 500 v D.C. at 0.1" gap Dielectric constant, 100C. 1000 cycle Dielectric Strength 25C.* Plash point, (C.O.C.)# Fixed Chlorine (Carius)* Specific heat at 25C.* Inorganic chlorides, ppm. TYPICAL 73 80, Seo. Saybold Universal 1.405 - 1.415 100 Max. Clear 0.01 max. .7 1.6285 - 1.6305 First drop 310C. min. 10# - 345C. Min. 90# - 385C. Max. 35 500 x 10 Ohm-cm., min. 4.6 35 KV min. 193C. 47.5 - 48.5# 0.27 0.10 max. *Not determined unless by special request. Hydrolysis Stability Test chlorides, ppm. Thermal Stability Test chlorides, ppm. 3.0 (tentative)^max. 0.5 (tentative) max. -66- Nv 007392 WATER PCB-00050960 AROCLOR 1254 PROPERTY Vise, at 98.9'C. (ASTM D88) ' Specific Gravity at 65/15*5#C. (ASTM D28?) Color, APHA Condition Acidity, mg.KOH/g. Pour Pt. *C. (ASTM D97) Inorganic Chlorides, ppm. Refractive Index at 25C. Distillation Range (ASTM D20) Corrected for stem and Barometric Pressure Corrosion TYPICAL . 44 - 48 sec. Saybolt Univer. 1.495 - 1.505 100 max. Clear 0.01 max. 7-12 No detectable amount 1.6370 - 1.6390 100 366 - 37oC. 500 371 - 383*C. 90# 379 - 394*C. After heating with aluminum for 6 hours at 210*C. plus or minus 10C. the aluminum must not be corroded either on visual or weight inspection and the Aroclor 1254 should meet the following specs: Color, APHA 150 max. Acidity, mg.KOH/g. 0.01 max. Free Chlorides,ppm. . No detec table amount Condition Clear Water Content, ppm. 35 max. Resistivity 100#C., 500 v D.C. at 0.1" gap 500 x 10^ ohm-cm., min. Dielectric Constant, 100C. 1000 cycles 4.15 - 4.35 Dielectric Strength, 25*C.* 35 KV, rain. Burn Point (ASTM D92)* Higher than 350*0. Sulfates (ASTM D-117-31)* None Fixed Chlorine Content (Carius)* Evaporation at 100'C. for 6 hrs.* 55 + 0.50 0.4jC max. Stability* There shall be no liberation of chlorine or chlorides when the material is heated at 100*C. in glass vessels in contact with air for periods of at least one month. Ageing Characteristics* No loss in resistivity over original value on heating in Specific Heat at 25*C.* air for 96'hrs. at 100*C. .0.26 ,v 1 *Not determined unless by special request. Hydrolysis Stability Test Chlorides, ppm. Thermal Stability Test Chlorides, ppm. 3.0 (tentative)max. 0.5 (tentative)max. NEV 007393 WATER PCB-00050961 AROCLOR 1260 PROPERTY TYPICAL Vise, at 98.9C. (ASTM D88) Specific Gravity at 90C./15.5C, (ASTM D287) Color, APHA Condition Acidity, mg.KOH/g. Pour Pt.,C.(ASTM D97) Inorganic chlorides, ppm. Refractive Index, 25C. Distillation Range (ASTM D20) Corrected for stem and barometric pressure. Corrosion 72 - 78 Sec. Saybolt Univ. 1.555 - 1.566 150 max. Clear 0.01 max, 25 - 34 No detectable amount 1.6455 - 1.6470 10 385 - 398C. 50# 390 - 404C. 90# 400 - 420C. After heating with aluminum for 6 hrs. at 210C. + 10C. the aluminum must not be cor roded either on visual or weight inspection and the Aroclor 1260 should meet the following specs: Water content, ppm. , Resistivity,100C. 500 volts at 0.1" gap Dielectric Strength 50C.* Dielectric Strength 100C.* Dielectric Constant 100C. at 1000 cycles* Burn Pt. (ASTM D92)* Sulfates (ASTM D117-31)* Fixed chlorine content (Carius)* Evaporation at 100C. for 6 hrs.* Stability* Specific Heat at 25C.* Color, APHA 150 max. Free Chlorides,ppm. No detec table amount. Acidity,mg.KOH/g. 0.01 max. Condition Clear 35 max. 500 x lO^ ohm--cm., min. 30 KV., min. 30 KV., min. 3.6 - 3.8 Higher than 350C. None 60 + 0.5# 0.2$ max. There shall be no liberation of chlorine or chlorides when the material is heated at 100C. in a glass vessel in contact with air for periods of at least one month. 0.23 *Not determined unless by special request. Hydrolysis Stability Test chlorides,ppm. Thermal Stability Test chlorides, ppm. 3.0 (tentative) max. 0.7 (tentative) max. -68- NEV 007394 WATER PCB-00050962 PYRANOL 1481 PROPERTIES Viscosity at 37.8*0. Spec. Gravity at 15.5/155C. Color, APHA Condition Acidity, mg. KOH/g. Pour Pt., *C. Inorganic Chlorides, ppm. Refractive Index at 25C. Distillation Range Corrected for stem and barometric pressure. First drop 25# max. 90# Corrosion Test Change in Weight Color, APHA Acidity, after test, mg.KOH/g. Free Chlorides, ppm. Condition after test Water Content, ppm. Resistivity at 100C 500 volts, DC, 0.1"gap Dielectric Constant (100C., 1000 cycles) Hydrolysis Stability Test chlorides, ppm. Thermal Stability Test chlorides, ppm. TYPICAL . 70 - 82 sec. Saybolt Univ. 1.525 - 1.535 150 max. Clear 0.01 max. -15 or lower 0.10 max. 1.6205 - 1.6215 205C. min. Below 270C. 380 - 395C. 0.0# 200 max. 0.01 max. 0.10 max. Clear 35 max. . 100 x 109 ohm"cm1min 4.1 - 4.6 3.0 (tentative) max. 0.5 (tentative) max. -69- NEV 007395 WATER PCB-00050963 PYRANOL 1488 PROPERTIES. TYPICAL Vise, at 37.8C. Spec. Grav. at 15.5/l5.5C. Color, APHA Acidity (Mg KOH/g) Water, ppm. Condition Refrac. Index at 25C. Free Chloride, ppm. Pour Point, C. Resis. at 100C., 500 v D.C. 1" gap Dielectric Strength (25C.) Corrosion: Loss of Aluminum 54-2 Sec. Saybolt Unlv. 1.560 - 1.568 150 max. .014 max. 35 max. Clear 1.6137 - 1.6147 0.10 max. ' Lower than -32C. 100 x 10^ ohm-cm min. Over 35 KV None Heating with aluminum for 6 hrs. at 200-220C. The Pyranol after heating should meet the following specs: Dielectric Constant at 1000 cycles at 100C.* Distilling Range (corrected)* 1st drop Below 270C. 90$ point Burn Point (ASTM D-92)* Fixed Chlorines* Arc Formed Gases* (Oxygen-free liquid at 25C.) Color, APHA Acidity (MgKOH/g) Free Chlorides ppm Condition 200 max. .014 max. .10 max. Clear 3.7 - 4.0 200C. min. 40$ max. 295 - 4l5C. None up to boiling point 59.1# min. Less than 1.0$ total com bustible gases including carbon monoxide, hydrogen, and volatile hydrocarbons. *Not determined unless by special request. -70- NEV 007396 WATER PCB-00050964 PYRANOL 1467 PROPERTIES TYPICAL Vise, at 37.8C., (ASTM D88) Specific Gravity at 15-5/15*5C. (ASTM D-287) Color, APHA Condition Acidity, mg. KOH/g. Pour Point, C. (ASTM D-97) Inorganic Chlorides, ppm. Refractive Index at 25C. Distillation Range (ASTM D20) Corrected for stem and barometric pressure Corrosion 54+2 sec. Saybolt Univ. 1.560 - 1.568 150 max. Clear 0.01 max. -32C. or lower 0.10 max. 1.6137 - 1.6147 1st drop - 200#C. min. Below 270C. - 40# max, 90# - 395 - 415C. After heating with aluminum for 6 hrs. at 200-220C., the aluminum must not be corroded either on visual or weight in spection and the Pyranol should meet the following specs: Color, APHA Acidity, mg.KOH/g. Inorganic Chlorides PPm. Condition 200 max. 0.01 max. 5 max. Clear WaterContent, ppm. Resistivity, 100C. 500 volts, 0.1" gap Dielectric Strength, 25#C. Dielectric Constant, 100C. 1000 cycles* Tin Tetraphenyl* Burn Point, (ASTM D92)* Fixed Chlorine* Arc Formed Gases* (Oxygen Free Liquid at 25C.) 30 max. 100 x 109 ohm-cm., min. 35 KV., min. 3.7 - 4.0 0.125# + 0.01# by weight None up to Boiling Point 59*1# min. Less than 1.0# Total combustible gases Including carbon monoxide, hydrogen and volatile hydro carbons. *Not determined unless by special request. -71- NEV 007397 WATER PCB-00050965 PYRANOL 1470 PROPERTIES TYPICAL Vise, at 37.8C. (ASTM D88) Spec. Gravity at 15.5/l5.56C., (ASTM D287) Color, APHA Condition Acidity, mg. KOH/g. Pour Pt., C., (ASTM D97) Inorganic Chlorides, ppm. Refractive Index at 25C. Distillation Range (ASTM D20) Corrected for stem and barometric pressure First drop 35# 55# 65$ 95$ Corrosion 41-45 Sec. Saybolt Unlv. 1.563 - 1.571 150 max. Clear' 0.01 max. -44C., or lower 0.10 max. 1.6075 - I.6085 210C., min. 240 - 256C. 290 - 330C. 385 - 400C. 395 - 415C. After heating with aluminum for 6 hrs. at 200-220C., the aluminum must not be corroded either on visual or weight inspection and the Pyranol should meet the following specs: Water Content, ppm. Resistivity, 100C., 500 v., 0.1"gap Dielectric Strength, 25C. Dielectric Constant, 100C., 1000 cycles# Tin Tetraphenyl* Burn Point, (ASTM D92)* Fixed Chlorine# Arc Formed Gases* (Oxygen Free Liquid at 25C.) Electrical Stability* Color, APHA Acidity, mg.KOH/g. Inorg.Chlorides,ppm Condition 30 max. 200 max. 0.01 max. 5 max. Clear 100 x 10^ ohm-cm., min. 35 KV., min. 3.8 - 4.3 0.125# 0.01# by weight None up to Boiling Point 60.5 0.5 Total combustible gases in cluding carbon monoxide, hydro gen and volatile hydrocarbons. After heating for 96 hrs. at 100C. in a closed container, the resistivity should not decrease more than 10#. *Not determined unless by special request. "72- NV 007398 WATER PCB-00050966 INERTEEN PPO PROPERTIES Vise. @ 37.8C., (ASTM D88) Specific Gravity @ 15.5/15.5C. (ASTM D-287) Color APHA Condition Acidity, mg. KOH/g. Pour point, C. (ASTM D-97) Inorganic Chlorides, ppm. Refractive Index @ 25C. Distillation range (ASTM D20) Corrected for stem and barometic pressure Corrosion Water content, ppm. Resist., 100C. 500 Volts, 0.1" gap Dielectric Strength, 25C. Dielectric constant, 100C. 1000 cycles* Phenoxy Propene Oxide or Glycidyl Phenyl Ether Burn point, (ASTM D92)* Fixed Chlorine* Arc formed gases* (Oxygen free liquid @ 25C*) TYPICAL 54- 2 sec. Saybolt Universal 1.560 - 1.568 150 max. Clear 0.014 max. -32C. or lower 0.10 max. 1.6137 - 1.6147 First drop - 200C. min. Below 270C. - 40$ max. 90$ - 395 - 4l5C. After heating with aluminum for 6 hours at 200 - 220C. the aluminum must not be corroded either on visual or weight inspection and the askarel should meet the follow ing specs: Color, APHA 200 rr..*x. Acidity, mg.KOH/g. 0.01*! r-- Inorganic Chlorides, ppm. 2 max. Condition Clear 30 max. 100 x 10 Ohm-cm., min. 35 KV., min. 3.7 - 4.0 0.1856 - O.2256 by weight None up to boiling point 59.156 min. Less than I.O56 Total combustible gases including carbon monoxide, hydrogen and volatile hydro carbons . *Not determined unless by special request. -73- NEV 007399 WATER PCB-00050967 CHAPTER 8 QUALITY REQUIREMENTS OF AROCLORS PRIOR TO USE IN THE ELECTRICAL INDUSTRY Quality as Supplied to the Electrical Industry Aroclors and their mixtures supplied to the electrical industry must meet the strict requirements specified by the industry and given in the specifications shown in Chapter 7. The electrical qualities, such as resistivity and power factor of the materials, as supplied, are not the maximum attainable. It is impractical for the manufacturer to furnish these dielectrics to the customer at the maximum attainable qualities because even with careful packaging, sampling, shipping, and handling, these fluids may pick up traces of contaminants from "clean" tank cars, drums, pipe lines, pumps, etc. However, as supplied in accordance with the specifications, the fluids must respond readily to "up-grading" by earth treatment to arrive at the desired maximum refinement required for use by the electrical industry. Typical Electrical Quality of Aroclors Used in the Industry Capacitor Impregnation Table IV indicates the desirable minimum resistivity values of Aroclor dielectrics immediately after earth refinement by the user when ready to impregnate capacitors. These values are compared with the similar values of the material after the capacitor impregnation has been completed in a relatively clean system. -74- Nev 007400 WATER PCB-00050968 TABLE IV Dielectric Volume Resistivity Ohm-cm at 100C. and 500 volts DC. Prior to After impregnation impregnation Aroclor 1254 2.500 x 10 800 x 10 Aroclor 1242 1.500 x 10 600 x 10 Pyranol l48l 600 x 10 400 x 10 The power factor of earth refined Aroclor prior to capacitor impregnation should not exceed 0.1 percent at 100C. and 1000 cycles, Transformer Filling The minimum resistivity of transformer askarel as specified for supply to the electrical industry is 100 x 10 Ohm-cm. at 100C., 500 volts and 0.1 inch gap. While power factor Is not part of the suppliers1 official specification, this value for freshly made transformer askarel ranges from 0.1 to 0.3 percent at 100C. and 1000 cycles. This would be approximately 0.05 percent at 20C. and 60 cycles. In order to arrive at higher and yet practical dielectric values the transformer manufacturer needs to earth refine the fluids immediately prior to using. It is reasonable to strive for a volume resistivity value around 1,500 x 10 Ohm-cm, at 100C. and power factor values of about 0.05 percent at 20C. and 60 cycles or 2 percent at 100C. and 60 cycles. -75-' NEV 007401 WATER PCB-00050969 Table V compares resistivity readings with the corres ponding power factor values obtained on the given samples of typical transformer askarel. TABLE V Volume Resistivity 10e Ohm-cm. at 100C. Power Factor 60 cy. 100*0. 60 cy. 20C. 1,500 2# 0.05# 500 5* 0.1# 100 15# 0.7# 60-70 20-25# 2.0# When adequately earth refined to give a resistivity in the range of 500 to 1500 x 10 Ohm-cm. at 100C., sample of such transformer askarel taken after filling a newly constructed and relatively clean transformer should have a resistivity of at least 200 x 10 Ohm-cm. at 100C. and a corresponding power factor less than 12 percent at 100C, and 60 cycles. -76- NV 007402 WATER PCB-00050970 CHAPTER 9 EARTH REFINEMENT OF AROCLORS TO ARRIVE AT THE DESIRED ELECTRICAL QUALITIES Earth Treatment In the Laboratory Preparatory to Analysis In Chapter 5 n Page 27 the laboratory procedure for preparing the test sample using 0.1 to 0.2 percent of activated earth Is given. It Is also stated that the absorbent Is minus 200 mesh Attapulgus earth' activated Just prior to use by heating in shallow trays for four hours at 400C. (752F.) or for at least 12 hours at 250C. (482F.) Earth Treatment by the Plant Manufacturing the Askarel Earth refinement in the plant is essentially the same as used when preparing the laboratory sample. The same amount of freshly conditioned earth (0.1 percent to 0.2 percent by weight) is added to the askarel and the mixture is agitated thoroughly and heated for about four hours. The more viscous dielectrics, such as Aroclor 1248 and Aroclor 1254 are heated at about 70 to 8oC. (158 to 176P.) and the less viscous materials such as Aroclor 1242 and Pyranols l48l, 1467 and 1470, or Inerteen PPO are heated at about 50 to 60C. (122 to 140P.) After about four hours contact the earth is removed from the dielectric fluids using a Sparkler or Sweetland or a comparable filter press, previously fitted with filter paper liners such as supplied by Carl Schleicher & Schuel Company, Inc., Keene, New Hampshire. The paper is usually 25 mils thick -77- NEV 007403 WATER PCB-00050971 and must be dried at 100C. to remove moisture prior to use in the filter press. Earth Refinement by the User Capacitor Manufacturers: Capacitor manufacturers usually use the same procedure for earth refining as employed by the manufacturer of the askarels. Because this method employs loose earth which can be thoroughly mixed into the askarel, it is believed to be the most efficient and is certainly known to give very good results. However, towers (cylinders) filled with relatively coarse earth through which the dielectric fluids are pumped and recirculated have also been used by capacitor manufacturers. Transformer Manufacturers: The large manufacturers of askarel transformers usually use the same type of procedure for refinement with loose earth as employed by the manufacturer of the askarel dielectrics. Handling relatively large amounts of the askarel transformer fluid Justifies installing the tanks and filter presses required. This earth refining equipment is . usually supplemented with portable cartridge type filters or a small portable platen frame type filter press. This latter equipment is then used when newly made askarel transformers are filled with the fluid and it is necessary to clean the transformer and the fluid by draining out the fluid pumping it through the filter press or cartridges containing the earth and recirculating until the desired electrical properties are attained. Likewise, smaller manufacturers of askarel transformers can use most conveniently the portable cartridge or platen frame type filters. ,,p N6V 007404 WATER PCB-00050972 t The Effect of Earth Refinement on Removal of Tin Teteraphenyl Scavengers from the Transformer Aakarel; As indicated above, normally transformer askarels respond readily to up-grading by the use of 0.1 to 0.2 percent by weight of earth based on the total weight of the fluid. However, if the fluids are unusually contaminated, larger amounts of earth are required to up-grade the dielectrics. This raises question about the selective adsorption of the scavengers by the earth treatment. It is indicated that to selectively adsorb significant amounts of the scavengers, repeated treatment with 1 percent or more of earth is required, as shown in the following table: TABLE VI REMOVAL OF TIN-TETRAPHENYL BY REPEATED TREATMENT OF ASKAREL WITH ONE PERCENT OF EARTH Sample No. Pyranol l4yo 1 Pyranol l4y0 2 Original O.II956 0.10756 Tln-tetraphenyl Content After 4 treatments After 7 treatments at 90C. at 90C. O.OI856 O.OO656 After 4 treatments After 6 treatments at 60C. at 60c. 0.02156 0.00356 -79- NEV 00 7405 WATER PCB-00050973 CHAPTER 10 ... CONTAMINATION Askarels as supplied by the manufacturer respond readily to earth refining resulting in a very high order of dielectric properties. For example, it is possible to attain volume resistivity values up to 20,000 or 30,000 x 10^ Ohm-Cm. at 100C., 500 volts, 0.1 inch gap and power factor values no more than 0.05# at 100C. and 1000 cycles. Except for very special situations, it Is not practical to refine these dielectrics to this extent. In commercial use, transfer of the fluids from one clean container to another which may result in contacting traces of conducting impurities does not allow maintaining such a high order of dielectric properties. Referring to electrical values, this accounts for the more practical order of specification values as indicated in Chapter 7 and to which the electric industry has committed the supplier of the dielectrics. This also aocounts for the desirability and need of the user of askarel dielectrics to earth refine Immediately prior to use in order to arrive at the maximum and yet practical dielectric values for his given purpose. Such quality values relative to askarels for capacitors and transformer work were Indicated in the preceding Chapter 8. AVOIDANCE OF CONTAMINATING ASKAREL CAPACITORS It is necessary, practical and economical that all steps possible be taken to avoid contaminating influences in the manu facture of askarel capacitors. -80- , Mtv 001-00 WATER PCB-00050974 I Sometimes capacitor manufacturers strive to attain the very | high order of dielectric qualities possible for askarel as mentioned above. Since it is very difficult, if not almost impossible to 1 { maintain such a high order, usually capacitor manufacturers comply I with the more practical schedule attainable by normal earth refining practices as shown in Table IV Chapter 8. | Equal care must be exercised in selecting, conditioning and handling the other construction materials of the askarel capacitor. i i For example, the water used in manufacturing capacitor tissue is , either distilled or deionized. Quality control of the capacitor ^ paper requires chemical tests to characterize the fiber and its J purity. Physical and electrical tests to determine moisture and power factor are essential. Acceptable dielectric loss values of | the dry and unimpregnated paper do not suffice for Judging quality , because in some instances after impregnation with good quality ' askarel, higher dielectric losses increasing rapidly with temperature | may be obtained. The aluminum foil used must be extremely pure and free from | residual traces of rolling oils or compounds. Accordingly, the ^ term usually applied to the foil Is "dry" foil. Similar care and 1 purity requirements apply to the aluminum tabs used. j The paper and aluminum foil is wound to form the core in an air conditioned room and often the machine operators are required | to wear cotton gloves to prevent oil from the operators skin contaminating the cores. " ' The steel cans or turn plate capacitor cans require thorough J cleansing and degreasing with perchloroethylene of required purity and free of any objectionable stabilizing agents. Similarly, the j -81 ' NEV 007407 WATER PCB-00050975 capacitor impregnating equipment and chambers must be kept clean. To facilitate maintenance of cleanliness, sometimes stainless steel construction is used. However, ordinary steel equipment is common and when "conditioned", that Is to say, coated with a thin film of clean Aroclor, this type of construction material is entirely satisfactory. To condition a new plant or clean an old one, askarel is circulated through the system, then purified by earth refining and recirculated. This process is repeated until all contaminating influences have been removed. Moisture, probably the most obvious contaminent in askarel impregnated capacitors, increases the dieleotrlc loss under AC voltage and decreases the capacitor life. Therefore, very efficient vacuum, as low as 5 or 10 microns, and heat carefully controlled up to 130C. are employed to expel the moisture from the capacitor cores prior to impregnation. Also to avoid moisture entering the askarel during storage, it is common practice to warm the dielectric in the storage tank to about 50C. in the presence of mild vacuum. Traces of any substances soluble in askarel and capable of ionization will have a marked adversed effect on the dielectric loss of the askarel or the finished capacitor. Therefore, much r care 1b required to avoid contamination with solder flux. For example, the use of rosin core solder is known to cause contamination. When rim sealing compounds are used in the lids of small capacitors, there must be assurance that the catalyst or other ingredients used in such materials do not cause contamination. Improperly selected pipe sealing compounds used on the threads on the fittings for sight glasses and instruments on the storage and impregnating equipment are known to have caused contamination. -82- nev fl oo?^a WATER PCB-00050976 #***#** All these factors about contamination must be kept In mind when Impregnating capacitors, especially by the chamber method but also by the manifold method. The moisture content of the paper used in the capacitor cores may easily introduce several gallons of water into the average impregnating chamber. This water is removed from the capacitors prior to impregnation -- usually by heating the chamber to 130C. in the presence of efficient vacuum, 100 microns or less. If the chamber is not made of the preferred materials of construction, slight corrosion (iron rusting) may occur and the film of askarel on the interior surface of the tank may become contaminated and introduce traces of Impurities into the clean dielectric fluid entering the chamber for impregnating the capacitors. In fact, because of this possibility of contamination, in some operations the capacitors are conditioned and dried in a separate oven or chamber. Then when thoroughly dried, they are then transferred into a second chamber used only for impregnation. In the case of relatively large sized capacitors, such as power factor correction units, a manifold with branches may be used to handle each unit Individually rather than by the batch -- chamber method. The unimpregnated capacitors are placed into an oven and vacuum is applied to the individual units attached to the manifold. After the capacitors have been evacuated and dried> the askarel is introduced through the manifold and its branches. Care must be taken that moist air or contaminants do not collect in the branches through which the dielectric is introduced. ******* -82A- NEV 007409 WATER PCB-00050977 Care must be taken to avoid contamination with any kind of grease, oil, packing material and "rubber" gaskets used with the machinery, such as pumps, etc., connected with the handling and impregnating facilities. It is not practical to discuss all possible sources of contamination and it should suffice to say that the manufacturers of askarel capacitors need to and do exercise all known precautions to avoid contamination and should evaluate and life test represent ative units before supplying the finished merchandise. AVOIDANCE OP CONTAMINATING ASKAREL TRANSFORMERS Obviously, in the manufacture of askarel transformers it is impractical and impossible to employ purification or refinements as required, for example, in the production of askarel power factor correction capacitors. In a transformer, heat from the dielectric losses of "slightly" contaminated askarel is negligible compared with heat generated by the transformer core. While power factor and resistivity of the transformer fluid are important, they are not as critical as is the case when Bimilar askarels are used in capacitors. However, this does not excuse the askarel transformer manufac turer from striving to meet the practical quality requirements as given in Chapter 8. In order to meet these requirements, it is necessary to earth refine the transformer askarel immediately prior to filling the unit. After the initial fill, the fluid should be withdrawn from the transformer, circulated through an earthen filter, then pumped back into the transformer and recirculated through the filter until both the fluid and transformer are clean and show the desired power factor and resistivity values, -83- NEV 007410 WATER PCB-00050978 If such normal earth refinement fails to give the desired results, it will be necessary to study the quality of the materials of construction and look for all possible sources of contamination in the transformer and handling equipment. The characteristic high dielectric strength of transformer askarel is not a good criterion of purity because with the exception of being adversely affected by moisture, it is not impaired irre spective of the contamination of soluble products which give increased power factor. F. M. Clark of General Electric Company tabulated the following values of transformer askarel selected from hundreds of askarel samples taken from commercially operating transformers to show lack of reduction of dielectric strength with marked increase of power factor values. TABLE VII DIELECTRIC STRENGTH AND POWER FACTORS OF ASKAREL IN USED TRANSFORMERS Sample Power Factor, 60 cy. at 25C., per oent Dielectric Strength at 25C. KV No. 1 0.1 38 No. 2 0.5 35 NO. 3 5 45 No. 4 15 39 No. 5 30 43 However, the need for care and proper selection of transformer construction materials is emphasized in the following tabulation which shows the marked increase of power factor resulting from contamination of the askarel with synthetic rubber materials and varnished cloth, as compared with acceptable materials of construction given in Table VIII. -84- NEV 007411 WATER PCB-00050979 TABLE VIII POWER FACTOR CONTAMINATION PRODUCED BY TRANSFORMER MATERIALS AGED IN ASKAREL AT 100C. FOR 96 HOURS Material None Black varniBhed cloth Askarel Power Factor, Percent 1.0 85.0 Dielectric Strength, KV 35 42 Copper Press Board Manila Paper Phenolic resin 1.5 40 2.0 37 1.5 39 1.6 41 Shellac 6.0 36 Iron 5.0 39 Synthetic rubber 70.0 39 Contaminants which cause a high power factor will of course also impair resistivity values, The following Table IX shows the degree to which acceptable and good commonly used materials of construction lower resistivity from the original high values possessed by the askarel. TABLE IX EFFECT OF COMMONLY USED INSULATION MATERIALS ON THE RESISTIVITY OF TRANSFORMER ASKAREL Sample gir-nmr-*---nr, Volume Resistivity x__ i> 108 Ohm. -cm. a,t q10A0OC^ . 1. Freshly made askarel before heat aging 2,000 2. Same as 1, after heat aging 1,900 3. After heat aging with the following materials added a - Phenolic resin tap changer material b - Paper c - Grade A press board (tan) 1,200 750 500 NEV 0Q7A12 WATER PCB-00050980 d - Grade A press board (gray) e - Grade A press board, laminated strip f - Cotton wrapping g - Glyptal 1276 cement, cured 48 hours at 110C. 500 400 300 100 The procedure used to evaluate materials of construction is simple and should be employed by all makers of askarel trans formers. One Inch square samples of the surface of the construction materials are immersed in one liter of good quality transformer askarel and heated for 96 hours at 100C. The increase in power factor and reduction of resistivity of the fluid after such exposure are compared with the values of the original fluid heated similarly but in the absence of the construction materials. The following Table X gives such a comparison and illustrates the unacceptable properties of the varnished cambric and black binding tape. TABLE X PROPERTY FRESHLY MADE TRANSFORMER ASKAREL SAME FLUID EXPOSED TO FIBER BOARD VARNISHED CAMBR! OR BLACK BINDINC TAPE PP, 100C., 1 KC Resistivity,ft100C. Ohm-cm. x 107 0.2% 2,500 0.45* 436 3% 18 Dielectric Strength at 25C. 45 KV 45 KV 45 KV When the askarel fluid contaminated with varnished cambric or the black binding tape was treated for one hour at 75C. with one percent by weight of attapulgua earth, the power factor and resistivlt values were restored to those of the original fluid. NEV 007413 WATER PCB-00050981 While there seem to be no reports of askarel transformers falling in service as a result of contamination from the use of questionable materials of construction, as discussed above, their unwise use is readily detectable and leads to embarrassing question about impairment of the transformer's life. Such a case is illustrated by an askarel transformer giving a megger reading reading as low as 3, after two years service life. The transformer had not been subjected to arcing and the dielectric strength of the askarel remained above 35 KV at 25C., or well within the specification of new askarel. Maintenance of high dielectric strength in the presence of contamination appears to account for the transformer not falling. The following Table XI compares the properties of freshly made askarel with the similar values of the fluid taken from the transformer after two years use and also with the same contaminated fluid following refinement by earth treatment. TABLE XI COMPARISON OP PROPERTIES OP CONTAMINATED TRANSFORMER ASKAREL BEFORE AND AFTER EARTH REFINEMENT PROPERTY TYPICAL OF NEW ASKAREL SAMPLE FROM TRANSFORMER USED 2 YEARS SAME SAMPLE AFTER EARTH TREATMENT 1 HOUR WITH 1# OF EART1 PF. 100C. 60'cycles * PF., 100C. 1 Kc. 1 to 2# 0.2* 150^(aissipation factor) 15# 1# 0.1# Resist. 100C. Ohm-cm. x 10 500 to 1500 ,, 6 ,, 2600 Dielectric Strength 25C. 45 Moisture ppm. 25 Acidity mg. KOH/g. 0.01 Color APHA 70 40 80 0 1000 -87- 45' 20 0.005 275 NEV 007414 WATER PCB-00050982 In the above case it was determined that a varnished insula ting material used in the transformer was the source of contamination Since this continuously dissolved in the askarel, obviously, removal of the fluid, followed by earth refinement and refilling the trans former accomplished nothing. The situation pertained at the time of the initial fill persisted until the deleterious component was removed. Newly built or rebuilt transformers using acceptable materials of construction often contain undeterminable traces of impurities and "dirt" which effect power factor and resistivity, but can be removed by repeated flushing with clean askarel. The following Table XII compares the properties of the askarel sampled after the initial fill with similar values after earth refinement and "soaking'' or flushing the transformer, twice with good askarel. After the "dirt" or contamination was removed from the transformer the askarel fluid remained in good condition in the unit as shown in Table XII. TABLE XII PROPERTY SAMPLE AS RECEIVED AFTER TREATMENT Resistivity @ 100C. 30 x 10 2600 x 10 Dielectric constant @ 100C. 3.9 3.9 Power Factor @ 100C., 1000 Cycles 2* 0.27* Moisture 60 ppm. 25 ppm. Moisture solubility in askarel at 25C. is about 110 parts per million and the specification for new askarel allows a maximum of 30 parts per million of water. Essentially, moisture-free askarel was found by Clark to have a dielectric strength of 70 KV. With increased amounts of dissolved -88- NEV 007^15 WATER PCB-00050983 water the dielectric strength gradually decreased and appeared to level off at a value of about 38 KV when the water content reached 80 parts per million. Water exceeding the solubility limit in askarel has a marked adverse affect on the power factor and resistivity of the dielectric fluid, which mey, however, maintain its high breakdown strength even though water accumulates as a separate phase on the surface. Undissolved moisture can be removed readily from transformer askarel by warming the fluid to 70C. and blowing with dry nitrogen or by treatment with dry, conditioned earth and filtering through a press fitted with dry filter papers or through an earthen cartridge type filter. As indicated previously, moisture must be kept out of askarel transformers by using adequate gaskets, as described in Chapter 3, and preferably sealing the device with dry nitrogen over the askarel. Mineral oil is soluble in these fire-resistant transformer askarels and is regarded to be a contaminant. Petroleum hydro carbons cannot be removed from askarels and the permissable amount may not exceed 2 percent by volume lest the fire-resistant values of the askarel is impaired beyond acceptable limits. Possible contaminants in transformer manufacture include welding and solder fluxes, oils and greases, bituminous materials, pipe thread lubricants, and contamination from bushing and pot head compounds. Paint or varnish coatings must not touch the interior of the transformer shell. Adhesives or coatings applied to gaskets must not touch the interior of the transformer. nev 007416 WATER PCB-00050984 All natural or synthetic rubber plastics or polymeric materials, resins, varnishes and lacquers and adhesives must be regarded as contaminants unless included in the very few acceptable classes and proved suitable by actual testing. . It is disappointing to find an askarel transformer manufacturer exercising precautions against contamination, and employing earth refinement, and yet inadvertently using a neoprene or other objectionable hose line to transfer the fluid economically!! If flexible hose needs be used, it should be a flexible stainless ' steel type or a "rubber" hose lined with Teflon. When using any of the following suggested suitable materials of construction, it is prudent to employ appropriate control evalua tion tests to be certain that the given material within a class regarded as acceptable will meet the requirements from a physical and electrical standpoint. TABLE XIII ACCEPTABLE MATERIAL FOR CONSTRUCTION OF ASKAREL TRANSFORMERS Structural Materials and Fillings Metals - Commonly used metals including steel, copper, aluminum, tin and brass are suitable if clean. Wood - Suitable if dry and free of natural gums and resins. Paper - Suitable ' Press Board - Suitable Cotton - Suitable Asbestos - Suitable Glass - Suitable Ceramics - Suitable Phenol-formaldehyde resins - Suitable if adequately cured. -90- NEV 007417 WATER PCB-00050985 Melamine-formaldehyde resins - Suitable if adequately cured. Cellulose acetate - Suitable Cellulose trl-acetate - Suitable Cork - Suitable Gasketing Materials and Adhesives Metals - (As above) Teflon - Suitable Silastic (silicone) - Suitable if adequately cured. Polyurethane - Suitable if adequately cured. Cork (fine grain and bonded with phenolic resin) - Suitable, but susceptible to penetration by askarel. Nitrile rubber - Sometimes used for gaskets - but susceptible to attack by askarel. Cork Nitrile rubber - Often used ' Dewaxed Orange Shellac - Suitable Epoxy - Suitable if adequately, cured. Isocyanate - Suitable if adequately cured. Tapes and Wire Insulation Cotton - Suitable Paper - Suitable Asbestos - Suitable . Glass - Suitable Rayon - Suitable Cellulose acetate - Suitable Teflon - Suitable Silicone - Suitable -91- Ngv 007^18 WATER PCB-00050986 Surface Coating for Transformer Exterior Baked Phenol-Formaldehyde - Suitable Baked Melamine-Formaldehyde - Suitable Baked Epoxies - Suitable Polyurethane Coatings - Suitable Surface Coating for Interior of Transformer Shell to Prevent Rusting In Storage 25 parts Aroclor 5460 dissolved in 75 parts lacquer thinner. ' The need for clean shop practice and avoidance of contaminating influences when building askarel transformers is emphasized by the ' following information submitted by a highly qualified manufacturer to indicate the condition of askarel sampled from normally opera ting apparatus after a number of years service. Fluid sampled from the top and bottom of at least 25 askarel transformers operatinj satisfactorily in different part of the country was analyzed, comprehensively. The following general conclusions were drawn: 1. The residual condition of the askarel samples for the most part was satisfactory, but in a few instances excessive dirt or sediment was noted. 2. Moisture content ranged from 19 to 6l parts per million with most samples between 25 and 35 ppm. Thio reflects a very good degree of dryness. 3. Acidity values were all below 0.01 mg. NaOH/g., which corresponds with the level of freshly made askarel. -92- NEV 007419 WATER PCB-00050987 4. In most cases the free chlorides did not exceed 0.1 ppm., the specification limit of new askarel. The highest reading was 0.15 ppm. 5. Dielectric strength values ranged from a maximum of 46 KV to a minimum of 28 KV which values are considred satisfactory. 6. Volume resistivity at 100C. ranged from 20 to 75 x 10 Ohm-cm. which is considered to be satisfactory and may be compared with the specification for new askarel at 100 x 10 Ohm-cm., minimum. 7. Power factor values at 100eC. and 60 cycles ranged from 19 to 75 percent with most samples below 60 percent. Prom the above data considered typical and satisfactory relative to all of these askarel transformers operating in a normal manner, it is seen that under satisfactory service life the resistivity of the askarel will decrease and the power factor will increase, as indicated, from similar values of fresh askarel. These observations emphasize the need for askarel transformer makers to: 1, Earth refine the askarel immediately prior to use in order to arrive at the highest practical electrical values from the fluid. 2. Avoid construction materials which are a source of contamlnat: 3. In using acceptable and satisfactorily tested construction materials - to flush the transformer to remove traces of contaminating influences and "dirt". 93" NEV 007420 WATER PCB-00050988 CHAPTER 11 REWORKING CONTAMINATED TRANSFORMER ASKAREL Normal Conditions Askarel contaminated during manufacture of the transformer or after years of normal service life should respond very readily to refinement by treatment with a few tenths of a percent of dry Fullers earth, or Attapulgus clay. This was discussed In detail In previous chapters. About askarel transformers, after years of normal service life and having continued satisfactory performance, question (difficult to answer) arises as to how high may be the power factor. Also, how low may be the volume resistivity. The case histories given in the preceding chapter seem helpful in arriving at an answer. DOble Engineering suggests to their clients that, "When used askarel is found to have a power factor of 2.0 percent or more, the cause of high power factor should be determined." (This refers to power factor measured at 20C. and 60 cycles.) Doble qualifies this suggestion stating, "If the high power factor is caused by water or other conducting matter, free chlorides or high neutralization number, the askarel is probably an operating hazard." Also, "If the high power factor is not due to these causes, it is probably not an operating hazard except that when the power factor is quite high, it may result in excessive heating of the device in which it is used." -94- NEV 007421 WATER PCB-00050989 Since heat resulting from power factor increase of the askarel in most any commercial transformer is negligible compared with heat generated by the core of the transformer, this consideration does not appear important. If the suggestion were limited to a 2 percent power factor, it would appear low and probably subject to considerable objection. However, when stated as 2 percent or more, the intention and purpose of this suggestion justifies earnest consideration, although in absence of more knowledge, it appears that conclusive answer to this question is not at hand. However, it should be apparent that when the power factor of the askarel is 2, 5, or 7 percent or higher at 20C. and 60 cycles, and volume resistivity at 100C. is 20 x 10 Ohm-cm. or lower, contamination is present. As it is likely that such a condition can be rectified by simple earth treatment and filtra tion, there should be little question about desirability of doing this purification work to assure the best possible perform ance of the transformer. Arced Conditions It is fortunate that there seem to be very few cases of significantly arced transformer askarel, as it is difficult to estimate the possible success of reclaiming the fluid. Particularly, it is not easy to lower the free and also the after corrosion chloride levels within the extremely low specification limits for new askarel. -95- oo2Z WATER PCB-00050990 Treatment with dry earth as usually used to refine contamina ted askarel, probably will not rectify arced askarel. Special refinement, including hydrolysis of the spent scavenger material, water extraction of excess chlorides, treatment with wet earth, special drying and finally treatment with dry earth is required. The following example is considered typical: During routine testing of a transformer filled with askarel, a short occurred in the winding, and the arc resulted in formation of easily seen carbon particles in the fluid. The following shows the ineffectiveness of dry earth treatment and the need for wet or water treatment to reclaim a sample of this material in the laboratory. Passing the damaged fluid through filter paper failed to remove the carbon. The carbon was removed by filtering through paper fitted with a one-half inch pad of Attapulgus earth. At this stage, analysis indicated the following pertinent properties as compared with the specification limits: PROPERTIES OF TRANSFORMER ASKARELS Specification Sample Inorganic chlorides Acidity, mg. KOH/g. Moisture 0.01 ppm. max. 0.010 max. 30 ppm. max. 0.25 ppm. 0.004 75 ppm. Then 0.2 percent by weight of Attapulgus earth was added and the mixture held at 90C. and agitated for two hours and filtered. This reduced the water to 15 ppm., but the chlorides remained at 0.25 ppm. Another portion of the original sample was treated' with 0.5 percent of earth, held at 50C. and agitated for two hours and filtered. This lower temperature treatment reduced the water to only 60 ppm. and the chlorides remained at 0.25 ppm. -96NEV 007423 WATER PCB-00050991 At this stage, the electrical properties were determined and found to be well within specification limits. Property Specification Sample Resistivity @ 100C. x 10 Ohm-cm. 100 576 Power Factor @ 100C. and 1,000 Cycles ------- 0.18# Dielectric Constant @ 100C. 3-8 - 4.3 4.2 The above reclaiming tests were repeated using "wet" earth which contained 15 percent moisture. Again, the chlorides remained at the original level of 0.25 ppm., well out of specification. Then a sample of the askarel was extracted with water, using 20 percent based on the weight of the dielectric fluid. This reduced the chlorides to 0.15 ppm., and a second aqueous extrac tion uBing 10 percent of water was required to reduce the chlorides to no detectable amount. The excess moisture was then removed by blowing with dry air and finally filtering through dry earth and filter paper. Although transformer askarel is several times as expensive as mineral oil, the material is not a'high cost item. Therefore, the economies of undertaking work as described above must be weighed against the cost of new askarel. In any event a fair estimate of the reclaiming cost plus . packaging, shipment to location for the work, the cost of several analyses involved, then repackaging in new containers and cost of return freight will indicate at least 50 percent of the cost of new askarel. Accordingly, usually the most practical expedient is to purchase new askarel to replace the arced material:. -97- NEV 007424 WATER PCB-00050992 CHAPTER 12 DERMATOLOGY AND TOXICOLOGY Skin Exposure Aroclors, or askarels, accidentally spilled on the skin do not cause an acute toxicity hazard, nor will they cause serious irritation. The materials should be washed from the skin with soap and water. Prolonged skin contact should be avoided. If work clothes become impregnated with these fluids, they should be removed and washed. When sampling tank cars, canvas gloves and safety glasses, or goggles, should be worn. No special clothing is required, but the workers' garments should be laundered at least weekly and changed, if Aroclors or askarels are spilled on the clothes. If accidental burns occur from contact with hot askarels, the burn should be treated the same as any ordinary burn. Aroclor, or askarel, adhering to the burned area need not be removed immediately unless treatment of the burn demands it in which case, soap and water, or repeated washings with a vegetable oil should be used. Accidental contact with the eyes results In painful irritation, but not permanent damage to the tissues or the sight. In event of such contact, the eyes should be flushed with a large amount of water for at least 15 minutes. The patient should then be referred to a physician who will treat with an ointment to soothe the eye. NEV 007425 WATER PCB-00050993 Exposure to Vapors Vapors from hot Aroclor, or askarel, have a degree of toxicity and should not be inhaled over a prolonged period of time. Experimental work on animals indicates that the maximum safe concentrations of vapors in work rooms is in the range of 0.5 to 1.0 mg. per cubic meter of air. Harmful amounts of the materials are readily detectable by odor and irritation to the eyes. Usually, people can detect concen trations of askarels in the amount of 1.0 mg. per cubic meter of air, which is the level regarded as the safe work room limit for an 8 hour day exposure. Capacitor impregnations may be done at temperatures as high as 266P. (130C.). Following impregnation and draining the chamber, exhaust ventilation should be applied to the chamber to prevent askarel vapors entering the work room. Also, when opening a heated capacitor impregnating chamber, the workmen should wear a respirator during this short Interval of exposure. If transformer askarels are used at temperatures above 125 to 150F. to fill an open transformer, exhaust ventilation should be provided in the immediate area. The many years of satisfactory and safe use of Aroclors, or askarels, by the electrical industry for impregnating capacitors and filling transformers has demonstrated the industry's ability to handle these fluids without hazard to the workmen. It is both simple and in line with "good housekeeping" and personal cleanliness to exercise the suggested precautions in all cases. -99- NEV 007426 WATER PCB-00050994 Vapors from a Severely Arced Askarel Transformer Experimental data indicate that when askarel is decomposed by an electric arc, insignificant amounts of chlorine and phosgene gas are liberated. The gas ia almost entirely hydrogen chloride, which is readily detectable by its odor and its irritating characteristics in even small amounts. Thereby, adequate warning of its presence Is provided and significant amounts of fumes would be likely to cause a hazard only in a closed area. Individuals would not voluntarily expose themselves to serious toxic levels of the hydrogen chloride gas fumes. ; -100- N6V 007427 WATER_PCB-00050995 g-5- BJ> IT 4 NV 00742b WATER PCB-00050996 NEV 007429 WATER PCB-00050997 OfT^ZOO A 3 M WATER_PCB-00050998 NEV 007431 i ! WATER_PCB-00050999 WATER PCB-00051000 ; /sc#<?/s f* v o c/ ff#P 02-f t <i NEV 007433 WATER PCB-00051001 NEV 007434 ?< /// WATER PCB-00051002 aintenance Guide & DEPOSITION ef EXHIBIT 2-(S' U NEV 007544 WATER_PCB-00051003 ASKAREL Inspection and Maintenance Guide * NEV 007545 WATER PCB-00051004 TABLE OF CONTENTS SECTION A TRANSFORMER ASKAREL Page I. Introduction........................................................................................................ I II. History of Trade Name Types........................................................................... I Tabic I -- The Composition of Transformer Askarels III. Table II -- Official Transformer Askarel Shipping Specifications................... A. General Electric Company's Transformer Pyranol A13B3B B. Westinghouse Transformer Inerteen PRO (7336-9) IV. Interchangeability and Stability......................................................................... 2-3 4 V. Directions For Handling and PersonalPrecautions............................................ 4 VI. Expected Service Life.......................................................................................... 5 VII. Dielectric Strength -- Moisture Relationship.................................................. A. Table III -- Dielectric Strength vs. Amount of Dissolved Water in Askarel and Mineral oil B. Table IV -- Approximate Solubility of Water in Askarel and Mineral Oil. 5 VIII. Table V -- Typical Values Found in Askarel Fluid Under Various Con ditions of Use..................................................................................................... 6 IX. Check Points For Maintaining Askarel Insulation........................................... A. General Considerations B. Modern Sealing Procedures C. The Older Sealing Arrangements 9 X. Periodic Fluid Inspection................................................................................... A. Visual Inspection B. Dielectric Strength II XI. Inspection Check List............................................................................... 12 XU. Contamination in Transformers...................................................................... A. Table VI -- Effect of Common Insulation Materials on Power Factor and Dielectric Strength B. Table VII -- Effect of Common Insulation Materials on VolumeResistivity 12 XIII. Refining Askarel For Re-Use........................................................................... A. Filtering Through Dry Blotter Paper To Remove Moisture and Extraneous Particles. Table VIII -- Guide to Rate of Dissolved Water Removal By Filtration. B. Earth Treatment for Maximum Improvement of Power Factor and Volume-Resistivity 1. Procedure 2. Effect of Earth on Removal of Scavengers 3. Table IX -- Approximate Relationship Between Power Factor, Volume-Resistivity and Dielectric Strength of Transformer Askarel 14 XIV. Cleaning Arced Transformers.......................................................................... 15 ' XV. Sampling ASKAREL......................................................................................... 17 NEV 007546 WATER PCB-00051005 SECTION B ASKAREL FILLED SWITCHES AND TERMINAL CHAMBERS Page I.Introduction.......................................................................................................... 18 II. Sources of Contamination.................................................................................. 18 III. Scaling Switches and Terminal Chambers........................................................ 19 IV. Askarel-filled Switches' Maintenance................................................................ 19 SECTION C Monsanto Analytical Services on Transformer Askarel.................................. 21 Appendix A. Askarel Stability and Composition of Arc Formed Gas................................ 23 B. Solubility of Gas in Transformer Askarel......................................................... 23 C. Approximate Vapor Pressure vs. Temperature ForTransformer Askarel____ 24 D. Effect of Temperature on Dielectric Strength of Askarel................................ 24 E. Viscosity of Askarel and Mineral Oil............................................................... 24 F. Density of Transformer Askarels...................................................................... 25 G. Thermal Conductivity........................................................................................ 25 H. Heat Capacity..................................................................................................... 25 I. Coefficient of Expansion.................................................................................... 25 J. Fire-Resistance.................................................................................................... 25 K. Seals, Properties and Procurement.................................................................... 26 NEV 007347 WATER PCB-00051006 SECTION A TRANSFORMER ASKAREL I. INTRODUCTION: This manual describes the operating characteristics of transformer ask are! liquid insulation and how it differs from mineral oil. The information given is based on facts gathered by Monsanto over 30 years as producer of askarel, plus knowledge gained from the experience of transformer manufacturers and users. This guide is provided to outline the very simple mainte nance required for askarel fluid in "modern" transformers and to offer suggestions for the sealing and maintaining of askarel in old units. By following this guide, users will obtain maximum service from askarel insulation with a reasonable minimum of maintenance. If questions arise relating to the designing and building of transformers -- these should be referred to regular transformer suppliers. Monsanto gratefully acknowledges the assistance, guidance, and the contributions of certain data by the following: Frank M. Clark. Edward L. Raab James G. Ford ., George Shombert, Jr, General Electric General Electric Westinghouse Electric ........... Allis Chalmers II. HISTORY OF TRADE NAME TYPES "Askarel" is the generic name for non-combustible (fire-resistant) liquid insulation. In this respect, the insulation is completely different from ordinary transformer mineral oils. Transformer askarel is marketed by Monsanto. Whatever the trade marked brand, the askarel contains Monsanto's Aroclor (chlorobiphenyl)... one of the best liquid insulations developed by science. This inert compound is chemically stable, fire-resistant, heat stable, non-corrosive, and has high dielectric strength under the operating conditions encountered in transformers. NEV 00754b WATER PCB-00051007 Askarcl liquid insulation is made by thinning Aroclor 1260 with trichlorobenzene or tri-, tetrachlorobenzene mix. The first transformer askarel was made in 1932, in accordance with General Electric Company's patents, and was trademarked Pyranol 1488. Westinghouse, loo, offered this askarel insulation in 1936 under their trademark Inerteen. In the mid-1940's, as shown in the following table, tin tetraphenyl was added to General Electric's Pyranol to scavenge hydrogen chloride. Shortly thereafter, Westinghouse added phenoxy propene oxide to Inerteen for the same purpose. In 1963, General Electric replaced tin tetraphenyl with a diepoxide scavenger. This new formula, which replaces previous Pyranols, is called Transformer Pyranol A13B3B. Thus, today the two commercial types offormulations arc General Electric s Transformer Pyranol AI3B3B type and Westinghouse Inerteen PPO (7336-9) type. The composition changes made in transformer askarel formulations arc shown in Table 1. Table I THE COMPOSITION OF TRANSFORMER ASKARELS 1488 Year Introduced....................... 1932 Ingredients: Aroclor 1260 ............................. Trichlorobenzene...................... Tetrachlorobenzene.............. Tin tetraphenyl.................... Phenoxy propene oxide........ Diepoxide.............................. 60 40 Pyranol 1467 1470 1944 1952 60 40 0.125 45 40 15 0.125 A13B3B Inerteen 1963 1936 45 60 40 40 15 0.125* III. Inerteen PPO (7336-9) 1945 60 40 0.20 OTHER BRAND NAMES Various electrical equipment manufacturers use other trade-marked names for askarel liquid insulation, such as Chlorextol (Allis-Chalmers); Noflamol (Wagner Electric); Saf-T-Kuhl (Kuhlman Electric). These askarel insulating liquids are one or the other of the two standard formulations. Still other manufacturers, who designate their insulation only by its generic name, askarel, assign it a number or code. By this number, Monsanto knows whether to furnish Pyranol A13B3B or Inerteen PPO (7336-9) type formulation to the user. III. OFFICIAL TRANSFORMER ASKAREL SHIPPING SPECIFICATIONS The official shipping specifications for the two modern transformer askarel formulations are shown in Table II. NEV 007549 WATER PCB-00051008 OFFICIAL TRANSFORMER ASKAREL SHIPPING SPECIFICATIONS General Electric Co. 9 3 NEW 007550 WATER PCB-00051009 IV. INTERCHANGEABILITY AND STABILITY A. Interchangeability: The two general types of askarel insulation shown in Table II can be either mixed or interchanged and there will be no difference in the operation of the transformer. However, askarel insulation must never be mixed with mineral oil. Over 2% mineral oil in askarel begins to lower its fire resistance. Further, materials of construction in the transformer that are compatible with askarel may not be compatible with oil and vice-versa. For example: a significant amount of askarel in a transformer built for mineral oil will attack gaskets, adhesives, core bindings, impregnating varnishes, etc. B. Stability: Askarel liquid insulation is highly pure, fire-proof liquid made under close chemical control. It does not vary in composition like the commercial range of mineral oils. Askarel does not deteriorate when exposed to air, heat, hot metal; it does not break down over long use to form conducting or corrosive chemicals; it does not oxidize or sludge. Askarel will remain perfectly stable year after year unless broken down by exposure to severe arcing. The only real "enemy" of askarel is contamination by water. Keeping askarel water-free will insure long-time service. Askarel is heavier than water. If water gets into askarel insulation, only a tiny amount (125 ppm) dissolves -- the rest floats on top. V. DIRECTIONS FOR HANDLING A. Keep Dry: In handling, storing, sampling, inspecting askarel -- and in operating askarel transformers -- take every precaution to guard the askarel insulation from exposure to high humidity and moisture contamination. Keep 5, 30, or 55 gallon drums of askarel dry; lay stored drums on their sides with the bung at the highest point from floor to keep water off the drum head (which can be sucked into the askarel by the drum "breathing"). This precaution is not necessary when drums are stored indoors, which is the preferred way of storing. B. Use Ordinary Personal Precautions: Transformer askarel has been made, handled, and used for over 30 years without causing toxic or other ill effects. It can be handled with only minor precautions. If accidentally spilled on hands, no serious skin irritation will occur. However, liquid askarel has a solvent action (similar to paint thinner) on the fats and oils of the skin and prolonged contact may lead to drying and chapping of the skin. *' NEV 007551 WATER PCB-00051010 In case of contact, wash off the skin with soap and water; remove and dry clean saturated clothing. Clean up spills with rags, sawdust or absorbent clay. Eye contact may result in painful irritation but no permanent damage to tissues. If askarel gets in the eyes, flush with large amounts of water. As with all eye first-aid, refer to a physician. To relieve irritation, physicians have used a 1% Pontocaine as well as opthalmic cortisone acetate solution, or castor oil. Infrequent exposure to askarel vapors will not cause ill effects. However, prolonged exposure to high vapor concentrations should be avoided. If hot askarel must be handled in a closed or confined area, provide the area with ordinary exhaust ventilation -- or -- wear an organic cartridge respirator approved by the U. S. Bureau of Mines. VI. EXPECTED SERVICE LIFE Properly designed and installed askarel transformers will give trouble-free service for a minimum of 30 years. Since their introduction in 1932, the manufacturers report finding the over-all failure rate to be less than 0.5% for all units under test and service conditions. The Edison Electric Institute's report (1956-1958) on their member utilities publishes the failure rate for askarel transformers as 0.13 per hundred banks per year. Even the rare reports of failure are invariably found to be due to improper sealing that allows moisture to enter. VII. DIELECTRIC STRENGTH -- MOISTURE RELATIONSHIP The dielectric strength of askarel is highly sensitive to excess moisture; not sensitive to ordinary dissolved contaminants. While the dielectric strength can also be lowered by severe arcing, askarel turns noticeably black or has particles of sooty carbon floating in it if arcing has occurred. Then the transformer should be repaired and the askarel replaced. New askarel has a minimum dielectric strength of 35 K.V at 25; a maximum mois ture content of 30 ppm. If the dielectric strength is checked periodically and decreases significantly -- this indicates moisture pick-up, arcing, or both. When the dielectric strength has dropped to 26 KV or less, an analysis for water is necessary. If water is found in excess of 100 ppm at 25 C., its source should be located and corrections made. When the moisture content approaches 125 ppm (saturation level), the dielectric strength of askarel drops below the value required for efficient insulating. The moisture content should not be allowed to rise over 70 ppm; it should be held as near as possible to 30 ppm. Maintaining a low moisture level will assure high dielectric strength and top operating efficiency. Table III shows the relationship of dielectric strength vs. moisture and Table IV indicates the approximate water solubility limits in askarel and mineral oil. . . 5 NEW 007552 WATER PCB-00051011 Table III RELATION OF "BREAKDOWN STRENGTH" TO AMOUNT OF DISSOLVED WATER IN ASKAREL AND MINERAL OIL Breakdown Voltage (ASTM) Water Content (PPM) Askarel Mineral Oil 0 70 KV 50 KV 20 55 39 40 47 30 60 40 26 80 38 22 110 10 5 Table IV APPROXIMATE SOLUBILITY OF WATER IN TRANSFORMER ASKAREL AND MINERAL OIL Temperature Amount of Water (PPM) Dissolved C. F. Askarel Mineral Oil --30 --20 --10 0 10 20 30 40 --22 _4 14 32 50 68 86 104 8 16 28 41 65 94 128 170 8 10 13 20 33 58 85 130 TURBIDITY . .. may be the visual sign of undissolved water, or may indicate contamination from core materials, dirt, or deteriorating construction materials. Cloudiness may also result from cold precipitation of tin telraphenyl "scavenger" that was used in the earlier Pyranols. This scavenger begins to come out of solution around I5F. above zero. To redissolve it requires heating to 150 - 200F. and agitation. High dielectric strength will quickly indicate that any turbidity present is not moisture; that the insulating efficiency of the askarel is still excellent. However, if the dielectric strength is below 26 KV, moisture should be determined, using the Karl Fischer method (ASTM D1533-60). The dielectric strength test for askarel serves primarily as an indicator for moisture. It is by far the most important maintenance test for transformer askarel. VIII. TYPICAL VALUES FOUND IN ASKAREL FLUID UNDER VARIOUS USE CONDITIONS Table V gives the entire spectrum of properties that are typical for freshly-made transformer askarel as it goes through the various normal and abnormal conditions of use. The data in Table V are in terms of only the askarelfluid and do not refer to insulation resistance or power factor measurements on the over-all transformer insulation. Several utilities studying the power factor values of the over-all transformer insulation system indicate that the unit power factor of a new askarel transformer should range from 1% to not over 5%. This would generally correspond with the askarel fluid properties as given under heading "B". 9 * NEV 007553 WATER PCB-00051012 TYPICAL VALUES FOUND IN ASKAREL FLUID UNDER VARIOUS CONDITIONS OF USE Dielect 2 5 X -, A properly b u ilt transformer is defined as one in which the materials o f construction are chemically and electrically compatible with askarel. 0a iP O3 4e0 . li.il I lilll $1 gO M U - II I6| .V5> .C5 C< ,, p 3 S 2 "g e fe T> ojS'j I K . g-s? li-s lls.l if I'sSh a i 8 e EIE a tc, "e 8c2O <'5 Si S. g1a to>c^TM *ofDcc,, ot ES -s3SCa gVjS < & ts c 11 n ilil S & e rs w ug a |JS aC0 cb V Sfl U 2 s-.g S 2 3-g zuiiS > * tn aM g g 0 fe 88 Beg 11 Si U1?. f5a. tK) O* E0 h u* w e ca EDQ., O > Ml 3 $ E2 3 If-K s!5 in c Jea & El t- e3 22 8^-gm 0 > * fi > * s I> * E3 E 'E E >Ml 2 K f*gs"*t * & K is? a i* FS S3 (N 6 sil^ s-82 " o is t$a$ a*? ^2 tv IN O e ft S& 0TM 'C O sM s 0 > *8 1J 11 K u && | 88 Uu | la Bo, " 0 7 NEV 007554 WATER PCB-00051013 Starting ideally with situation "B", it is normal to expect the power factor of the fluid in a satisfactorily operating ask arc! transformer to increase as shown under heading "C". The "over-all" power factor of the transformer in normal service is expected to rise, but preferably not much beyond 5%. In this normal situation, the moisture level of the askarel fluid and its dielectric strength will be satisfactory, as shown in heading "C". Occasionally the power factor of a non-arced, satisfactorily-operating askarel transformer is found to be relatively high, i.e., 15%. In this case, the power factor of the askarel fluid wilt also he high, perhaps as high as 50% at 20C. and 60 cycles. It is not good practice merely to note that high power factor of the askarel fluid is to be expected. The important step is to check dielectric strength and note whether there has been a downward trend. A downward trend in dielectric strength very likely indicates moisture entrance and should be confirmed by a Karl Fischer test for water. The importance of any abnormalities in dielectric strength and moisture content of the askarel fluid cannot be overemphasized! Where abnormal values for the dielec tric strength or moisture content occur, the power factor of the transformer can be expected to be abnormally high; the expected high power factor of the askarel fluid will induce this. The indication (hat a high power factor on the transformer and on the fluid is due to contamination can be verified by earth refining the askarel fluid and noting whether after refining the test results correspond with heading "C". Assuming no mechanical defect or arcing, if the power factor of a new askarel transformer is relatively high, the power factor of the fluid will also be high, giving the situation under heading "D". This reflects contamination that should have been removed by the manufacturer of the transformer. In absence of mechanical defect, where there are no abnormal losses in dielectric strength, and no moisture pick-up in non-arced askarel -- the use history shows that a relatively high power factor for the askarel fluid (as compared with mineral oil) is to be expected. Normally, high power factor is due to contamination and not deterioration of the askarel operation. As shown by F. M. Clark in his book, "Insulating Materials For Design and Engineering Practice," John Wiley & Sons, N. Y., 1962 -- activated alumina can be used in the circulating system to bring the power factor down and keep it as low as possible. 0 NEV 007555 WATER PCB-00051014 IX. CHECK POINTS FOR MAINTAINING ASKAREL INSULATION A. General Considerations; Modern askarel transformers with welded construction or silicone gaskets for hand hole-cover, switch and terminal compartment covers, with properly constructed bushings require little or no maintenance. With properly con structed transformers, annual or semi-annual visual inspection and dielectric strength test of the askarel fluid should suffice for routine maintenance checking over many years of service. However, many askarel units were installed in the early 1930's -- before the development of some of the better modern gasketing materials and before improved designs were developed for sealing out moisture. Such early units should be, and can be, modernized. Leaky or deteriorated gaskets should be replaced. If the askarel has become contaminated, it should be reconditioned. At the, same time, a general clean-up of the unit and possible refinishing may be desirable. If it is not convenient to take an old transformer out of service for general repairs, leaky gaskets can be sealed temporarily by painting over the leaky area with epoxy cement. A survey of users indicates a good number of early-built askarel transformers (over 20 years old) are kept in continuous service in critical installations by the following steps (instead of modernization). The operating units are equipped with compound pressure gauges for reading pressure above and below atmospheric. Positive pressure is maintained on the shell by introducing nitrogen at 2 to 3 pounds above atomspheric. Regular workmen in the area daily record the temperature and pressure. If a sudend pressure drop is noted more nitrogen is introduced and the gaskets are checked for leaks with soap solution. Leaks are sealed by applying epoxy cement. B. Modern Sealing Procedures; Transformer purchasers should specify the following modern techniques for sealing; 1. Welding Construction: Covers, radiator connections, switch and terminal housings, instrument connections, etc. should be welded. 2. Bushing Connections: The most satisfactory bushings are the type with rolled-on flanges and two ring seals rolled into a depression in the porcelain -- scaled with silicone rubber rings held under compression. Metal-to-glass or metal-to-porcelain sealed bushings are also satisfactory. If for any reason the above type bushings cannot be used then use a por celain or glass bushing with a silicone or Viton gasket retained in a groove. The gasket can be either rectangular or circular cross section, usually % inch thick. 3. Small Size Connections; When not possible to weld, small size connection seals should be made with Flexitallic stainless steel rings. The surfaces must be machined and parallel. The filler between the steel laminations of the Flexitallic ring should be either silicone or Viton. * # 9 NEW 007556 WATER PCB-00051015 4. Gaskets For Hand-Hole Covers: Modern design specifies silicone gaskets. Such gaskets must be retained in a groove. The groove preferably is machined into the flange or cover. However, it can also be formed by welding concentric steel strips to the flange or the cover. Generally the gaskets should be s/l9 to V4 inch thick for covers, depending on the depth of the groove. A rectangular section is usually used. The silicone material should be Dow-Corning No. 50 Silastic or equivalent. This is a low compression set material. For best sealing 20 to 25% compres sion is recommended, with ample clearance in the groove to allow for th's compression. No cement is required. With reasonable care the gasket is removable without damage and is reusable. Silastic 50 is slightly swelled by askarel which contributes to the tightness of the seal. It is not deteriorated by askarel fluid or vapors. It resists weather ing and it is thermally stable and flexible at all operating temperatures. It is an excellent moisture barrier. Notes: a. Dow-Corning, Midland, Michigan will supply a list of Silastic 50 gasket fabricators to all transformer manufacturers or users. They will also furnish technical data. b. Any user of Pyranol transformers, made by General Electric Company at Rome, Ga., will receive prompt and generous help for converting to the modern silicone or Viton gaskets by contacting the General Electric Company's Service Engineering Department at Rome, Ga. See Appendix K: Seals, Properties and Procurements. C. The Older Sealing Arrangements: The older type gaskets consist of either cork or cork-nitrile rubber combinations or straight nitrile rubber. 1. Cork-Nitrile Combinations: Covers for the main tank, hand-holes, switch and terminal chambers, relief diaphrams etc. are held in place by studs welded to the flange or by bolts. The gaskets are cut with openings and placed over the bolts. Often Shellac (Westinghouse Style No. 1150419, or General Electric Company's Glyptal 1276) is used to cement the cork to the flanges. The following is recommended for scaling with (he cork -- nitrile rubber combination: Use Armstrong NC-757 cork-nitrile material or equivalent. The gasket can be cut from a single sheet or by scarfing strips of the material. A convenient method for joining strips is to make a Keystone Type joint. For this. Westinghouse, Sharon, Pa., offers their gasket cutter Style No. 328 B6I4 G01, (about SI5). The joints should be cemented and the gasket also cemented to the flange, using one of the above cements. Excess cement should not be allowed to reach the interior of the transformer. ,. # 10 NEV 007557 I I WATER PCB-00051016 After installation and bolting, the outside edge of the gasket should be coated thoroughly with epoxy cement to increase weather resistance. This epoxy cement is a paste to which a curing catalyst is added immediately before use. Typical are: a. Epoxy Patch Kit ff!-C Hysol Corporation, Olean, N. Y. b. Scotchcast Resin tf4 Minnesota Mining and Manufacturing Co. St. Paul, Minnesota c. Adhesive A-J and Activator Type B Armstrong Products Company Argonne Rd., Warsaw, Ind. d. Adhesive 9860-1, Synthetics Organic Company, Cleveland, Ohio, used with activator diethylene triamine (Carbide and Carbon Chem. Co.) 2. Straight Nitrile Rubber: When straight nitrile rubber was originally used, invariably the gasket was recessed in a groove. This was to prevent gasket flow and to protect the material against excessive compression. Although this type seal was not cemented, the nitrile rubber gasket is not reuseable. Since grooves or stops have already been provided for the nitrile rubber seal, Silastic 50 can be easily substituted and is recommended. This conforms with modern practice. X. PERIODIC FLUID INSPECTION AND WHAT CHECKPOINTS MEAN On a regular schedule -- at six, nine, or twelve month intervals -- make a simple visual inspection of your askarel insulation and run a dielectric strength check. A. Visual Inspection: Askarel is a clear, faint-yellow liquid. After long-term use this color may gradually intensify to light brown. The fluid should remain clear and free from turbidity or cloudiness. Any color change -- such as to a green, red or blue cast -- indicates extraction of impurities from the solid insulation. If a distinct foreign color pick-up is noted, check the complete range of electrical characteristics and notify the transformer maker. The electrical characteristics may be found to be unim paired. Color change alone (except for black) is not a danger signal since the contamination is not likely to impair the dielectric strength. B. Dielectric Strength: < If the dielectric strength has decreased significantly from the last inspection, or if it has gradually decreased below 26 KV range (at 25C.) -- RUN A CHECK FOR MOISTURE. Use ASTM D901, D877 (Karl Fischer Method). The dielectric strength of askarel is the major indicator to the operating efficiency of your liquid insulation and of the askarel transformer itself. Besides the "visual" inspection tests, dielectric strength is the only test necessary to run on a routine basis. Well-sealed askarel transformers have service records of 25 to 30 years on the original askarel. New askarel has a minimum dielectric strength of 35 KV at 35C., a maximum moisture content of 30 ppm. NEV 007558 WATER PCB-00051017 XL INSPECTION CHECK LIST 1. If askarel is clear, even though darkened to light brown; has no sediment or turbidity; has dielectric strength over 26 KV.. . give it the inspection "OK''. 2. If askarel is clear; has foreign color of blue, green, red . .. it is "extracting color" from internal materials. This is not,of itself, an operating hazard when the dielectric strength stays over 26 KV and moisture remains low. However, this rare occur rence calls for checking into condition of the interior construction and consulting the transformer maker. 3. If askarel is clear; but dielectric strength drops to 22 or lower KV, and moisture rises over 80 ppm .. . the askarel is ready for simple "refining". If the moisture is near the saturation level (about 125 ppm), a thorough inspection should be made for water droplets in the transformer tank, and even for "globules" or water floating on the askarel surface. If found, the transformer manufacturer should be consulted for reconditioning both the transformer and the fluid. 4. If askarel is dark brown to black; if black particles of carbon are seen; and dielectric strength is low... the askarel has been broken down by arcing. It cannot be refined and should be discarded. If any of these four simple inspection tests appear out of the ordinary, or the relationship between appearance and test values is abnormal -- contact your transformer supplier for a complete analysis. Whenever a sample is to be shipped to Monsanto, please follow the directions shown under: "SAMPLING ASKAREL". . XII. CONTAMINATION IN TRANSFORMERS Unlike mineral oil which can oxidize, sludge and deteriorate -- askarel breaks down in transformer use only when strongly arced. Thus, while askarel does not decompose in normal use -- it can be contaminated more readily than the relatively non-polar mineral oil. For example the following Table VI shows how a small amount of synthetic rubber or a bit of varnished cloth markedly increases the power factor of the askarel. Please note, however, that such minor contamination has no adverse effect on the dielectric strength. As explained, moisture entrance through faulty seals seems the only contaminant in normal use that lowers the dielectric strength of transformer askarel. 12 NV 007559 WATER PCB-00051018 Table VI EFFECT OF COMMON INSULATION MATERIALS ON POWER FACTOR AND DIELECTRIC STRENGTH (HEAT AGED 96 HOURS IN ASKAREL AT I00C.) Material Immersed None (control)............................................ .. Black varnished cloth................................ .. Copper......................................................... .. Pressboard................................................... .. Manila paper.............................................. .. Phenol formaldehyde resins...................... .. Shellac..................................... .................... .. Iron.............................................................. .. Synthetic rubber......................................... .. Askarel After Exposure Power Factor, Percent at 60 eye., I00C. Dielectric Strength 25C. 1.0 85.0 1.5 2.0 1.5 1.6 6.0 5.0 70.0 35 KV 42 40 37 39 41 36 39 39 Similarly, trace contaminants from commonly used construction materials can lower the volume - resistivity of askarel, without affecting its dielectric strength. Table VII shows this. Table VII EFFECT OF COMMON INSULATION MATERIALS ON VOLUME RESISTIVITY OF ASKAREL Sample i. New askarel before heat aging...................................... 2. New askarel after heat aging 96 hours at I00C........... 3. After heat aging with 1 sq. inch specimens of: a. Phenolic resin tap changer material........................ b. Paper............................................................................ c. Grade A press board (tan)........................................ d. Grade A press board (gray)...................................... e. Grade A press board, laminated strip..................... f. Cotton wrapping........................ ................................ g. Glyptal 1276 cement, cured 48 hrs. at II0*C.......... Volume Resistivity x 10* ohm-cm (at I00C., 500 Volts DC., 0.1* gap) 2,000 1,900 1,200 750 500 500 400 300 100 While trace contamination easily lowers volume resistivity from high levels, it is important as previously noted in Table V Case F, that heavy contamination (as when arced) does not lower the resistivity below the order of SO' ohm-cm. at 100C. The different behavior of askarel vs. mineral oil in these respects can be summarized as follows: High power factor and low volume resistivity in transformer mineral oils are commonly regarded as "danger signals" that the oil has deteriorated and broken down chemically. This is NOT TRUE of askarel liquid insulation, unless the dielectric strength is low. NEV 007560 WATER_PCB-00051019 XIII. REFINING ASKAREL FOR RE-USE A. Filtering Through Dry Blotter Paper to Remove Moisture and Extraneous Partciles: Most operators prefer portable refining apparatus, such as a plate press filled . with a dolly, (available from Sparkler, Mundelein, III., Westinghouse Main tenance and Repair Dept., Chicago, or General Electric Co., Pittsfield, Mass.); or the earthen cartridge filter type, (available from Industrial Filter Corp., Lebanon, Ind.). Filter paper liners for the plate press are available from Carl Schleicher and Schuell Company, Keane, New Hampshire and manufacturers of filter presses listed above. The filter paper must be dried immediately before use. For best results, spread the paper for maximum surface exposure in a hot air circulating oven and heat it for 4 to 6 hours at I lO^C. If possible do not take the transformer out of service until ready to filter the fluid. This will keep the transformer coils relatively hot and dry. Processing the fluid should start immediately after de-energizing the unit. Circulate the askarel hot (but not over 55-606C.) through the filter fitted with the dry paper liners. After filtration the dielectric strength of the askarel should be 35 KV minimum. 1, Precautions: Filtering should not be done when the relative humidity exceeds 75%. 2, Any flexible hoses and gaskets on the refining equipment should be lined with or made of materials that will not be softened by contact with askarel fluid. (Silicone or Teflon-lined, or flexible metal materials are suitable.) Table VIII GUIDE TO RATE OF DISSOLVED WATER REMOVAL BV FILTERING ASKAREL THROUGH A PAPER PRESS Pams Throagb Paper Prew 0 1 2 3 4 3 6 Water So Aikarel PPM IIS 35 22 18 12 10 to heV 007561 WATER_PCB B. Earth Treatment for Maximum Improvement of Power Factor and VolumeResistivity: 1. Procedure: (The askarel liquid should be relatively dry prior to the following earth filtration.) Use finely divided Attapulgus clay or Fuller's earth (dried and activated by healing for 12 hours at 300-350F. immediately prior to use) as a coating on the filter paper surface. The amount of earth used should be 0.1 to 0.2 per cent by weight on the weight of the askarel to be treated. (Askarel weighs about 13 pounds per gallon). To deposit the earth evenly, stir one-third of the earth with a small portion of askarel in a clean container. Pump the mixture through the filter and follow with two more one-third portions. Then circulate askarel taken from near the top of the transformer, pass it hot (not over 55-60C.) through the earth coated filter and feed back through the bottom transformer outlet. Continue circulation until the fluid is clear and test shows that the electrical properties are fully restored. 2. Effect of Earth on Removal of Scavengers: Only slight and insignificant loss (by selective absorption) of tinletraphenyl and epoxides occurs when askarel is refined by treatment with 0.1 to 0.2 per cent by weight ofearth. To remove significant amounts of the scavengers requires repetitious treatment with much larger amounts of earth. 3. Table IX -- Approximate Relationship Between Power Factor, Volume Resistivity and Dielectric Strength of Transformer Askarel: Power Factor (60 eye.) tore. 25C. 2% 5% 15% 0.05% 0.1% 0.7% 20-25% 2.0% 40-50% -- Volume Resistivity x 10 ohm-cm. (at 100C., 500 Volts DC., 0,1' gap) 1500 500 100 60-70 25 Dielectric Strength 25C., 0.1' gap 35 KV 35 35 35 35 If it is desired (although these factors are not generally considered important for askarel transformers), to keep the power factor as low as possible and the resistivity as high as possible, hang a container of anhydrous alumina or activated clay in the circulating system of the transformer. XIV. CLEANING ARCED TRANSFORMERS If a unit has arced so that the askarel is no longer fit for use, a thorough cleaning of the unit is necessary before refilling with new askarel insulation and returning it to service*. Follow this procedure: . 15 NEV 007&62 WATER PCB-00051021 A. Drain out all dark, carbon-contaminated askarel. (Discard by dumping or burying where it will not contaminate a water supply.) B. Carefully brush carbon deposits from internal parts and insulation, using a soft bristle brush making sure that insulation is not damaged. C. Flush thoroughly using new askarel (not an oil, not a cleaning solvent). D. Flush a second time with fresh askarel; drain; then fill to the proper level with new askarel. E. Energize transformer to warm the fluid for 24 to 48 hours; then circulate the askarel through a filter, returning it to the unit filtered and ready for use. This assumes that the cause of arcing has been established and corrections made. When severe arcing occurs, major repairs are usually necessary and the unit rebuilt. This procedure can be applied for flushing out repaired units. NEV 007563 WATER_PCB-00051022 XV. SAMPLING ASKAREL Take a sample as close to the top of the liquid surface as possible. (Many large askarel transformers have a built-in sampling tube near the surface for convenient sampling). Then, to make sure that your SAMPLE truly represents your askarel insulation, take another sample from the bottom. If additional sampling tube connections are contrived on the valves for easier sampling, make the tubes of clean glass, stainless steel, aluminum or tin for rigid types; and silicone or Teflon tubing for flexible types. Use NEW containers for the askarel sample. A new and thoroughly pre-dried smallmouth quart glass bottle fitted with a Bakelite screw cap fitted with an aluminum or (in bottle cap liner is recommended for "quick on-the-site testing." (If complete analysis is to be made, a 5-pint size sample is required). Be sure that the new bottle does not stand open to collect dust or moisture. Rinse the sample bottle and cap lining two or three times with askarel from the transformer; then fill it. If the sample will be tested promptly, a clear glass bottle can be used. If sample is to be stored indefinitely, use an amber glass bottle or wrap clear glass with aluminum foil. A. Select a dry day. Do not sample insulation on a warm, moist day when humidity exceeds 75%, and ... B. Make sure that the askarel is at least as warm as the surrounding air. (Cold liquids can condense moisture from humid air.) C. When sampling askarel from transformers, it is best to take the sample when the unit is warm and operating at average or maximum load. Especially as a check on moisture (as reflected by a dielectric strength test), sampling the warm askarel more truly represents its condition during operation. Experience shows that water will migrate from a transformer's solid insulation to the askarel liquid and vice versa, depending on temperature. Therefore, when the transformer is hot, the moisture is most likely to be found in the liquid. This accounts largely for periodic variations in dielectric strength. For example: a relatively high dielectric strength may be found during winter months and a relatively low dielectric strength during the summer months on samples taken from the same unit. 17 NEV 00?&6<r WATER PCB-00051023 SECTION B ASKAREL FILLED SWITCHES AND TERMINAL CHAMBERS I. INTRODUCTION: High voltage leads are usually connected to askarel or mineral oil-filled network transformers and power centers through terminal chambers and switches. In some cases terminal chambers are not used, and the high voltage leads are connected directly to the switch terminals. They may be filled with either askarel or mineral oil. Switches are usually rotary or drum type fitted with a revolving block and porcelain unit as the principal element arranged for three-phase service. (A cutaway view of a typical terminal chamber-switch combination is shown for reference.) Askarel transformers with attached switches have been in use for about 30 years. When they were first introduced, the availability of insulating and gasketing materials was rather limited and even the best materials at the time had no service history. As a result, inadequate gasketing materials such as cork, nitrile rubber, and nitrile rubbcr-and-cork particles were used. While satisfactory for a limited period of time, these materials cannot be depended on for the expected long life of the equipment. The terminal chamber is usually above or below the switch compartment and separated by a steel wall through which the bushings are inserted. When bushings are properly selected and correctly installed, there is no leakage from one compart ment to the other. With poor bushing seals, and the terminal chamber above the switch, potting compounds or cable oil can seep into the askarel. When the terminal chamber is below the switch, askarel can drain into the terminal chamber. II. SOURCES OF CONTAMINATION There are three possible sources of contamination for askarel in switches and terminal chambers; they rank in this order of frequency: (I) water entering through poor gaskets; (2) decomposition products from arcing when switch is used to break magnetizing current; (3) entrance of pothead or cable compounds through leaky bushing seals. Unlike an askarel transformer where the amount of contaminant is likely to be very small (probably only trace amounts) in relation to the volume of askarel fluid -- in switches or terminal chambers with faulty seals, the amount of contamination can be relatively large. *' NEV 007565 WATER_PCB-00051024 Experience has shown that, based on the number of installed askarel-switch units, the percentage of failures is extremely small. When investigated, it has been found that most failures originate in the switch chamber. Water is the chief source of contamination. However, heavy contamination of askarel with petrolatum and asphalt material, due to leakage, have caused a few failures. Petrolatum is used frequently for filling terminal chambers. When either cable oil or petrolatum seeps into askarel, no great harm results. The fire resistance will be somewhat decreased and power factor of the askarel will increase with an accom panying drop in resistivity. While highly undesirable, it is doubtful that failure of the unit results. Where asphaltic compounds are used in place of petrolatum, the danger is increased somewhat because asphaltic contamination may cause exces sively high dielectric losses in the askarel. When the terminal chamber is below the switch chamber, the potting compound can be contaminated by askarel if the bushing seals are leaky. This is undesirable because the askarel will increase the power factor and conductivity of the potting compound or cable oil and develop heat from dielectric loss. If this mixture is drawn into the cable insulation, a cable failure is likely. This again emphasizes the impor tance of tight bushing assemblies. III. SEALING SWITCHES AND TERMINAL CHAMBERS Proper bushing construction, use of Silastic seals and welding wherever possible is highly desirable (as covered in Section A). Where an elastomeric seal is to be used in contact with both askarel and petroleum oil, DuPont's Viton is suggested. For new equipment the user should specify these modern sealing arrangements to keep out contaminants and minimize maintenance. IV. MAINTENANCE FOR ASKAREL FILLED SWITCHES A. Switches used for grounding after power source has been de-energized will not undergo arcing. B. Switches interrupting magnetizing current will be subject to arcing; the amount of decomposition will depend on power interrupted, time and frequency of oper ation. As a general rule, the liquid should be checked after 5 to 10 operations. NEV 007566 19 WATER PCB-00051025 1. On newly installed switches, check the askarel at 3,6 and 12 month intervals; if found satisfactory, check once annually thereafter. With proper attention to the gasketing of covers and bushings, experience will probably indicate that less frequent inspection is warranted. 2. Check askarel for: a. Dielectric strength (ASTM D877): It should be 26 KV minimum. If dielectric strength is low, confirm presence of water by Karl Fischer method ASTM D-1533. Filter to remove moisture. Dielectric strength should then be 30 KV minimum. b. Presence of carbon from arcing; Fluid should be relatively free of carbon. If badly arced and very black, replace fluid. If only minute amounts of carbon are present, filtration is recommended. Check power factor of liquid (should not be over 5% at 25C. and 60 cycles). Flush out switch chamber with several gallons of fresh askarel before refilling. 3. If there is discoloration, high power factor, detectable change in specific gravity or refractive index, or if fluid flashes below 250F., there is a possibility of seepage of potting compound into the switch compartment. In this case, correct any leaky bushing seals with proper replacements and fill with new askarel. 4. If terminal chamber is below switch, check potting compound for presence of askarel (can usually be detected by odor or by an increase in specific gravity). If askarel is present, correct any leaky bushing seals with proper replacements, and renew compounds. 5. Examine cover gaskets visually. Deterioration can be detected by swelling and cracking of the exposed edge. In cases of severe deterioration, liquid seepage is usually present. 6. Check for leakage at packing gland of switching shaft. If leaking, repack with a Silastic ring type gasket. # 20 NV 007567 WATER PCB-00051026 SECTION C ANALYTICAL SERVICES ON TRANSFORMER ASKAREL AVAILABLE FROM MONSANTO Transformer users not wishing to make their own fluid analyses can obtain the service from Monsanto. Simply contact Monsanto and specify what analyses are wanted. You will be sent the proper-sized sample container filled with fresh askarel. When you receive this, empty it and carefully take your sample (following the procedure for sampling in this guide). Send the container to Monsanto's laboratory. Charges listed include sample container, shipping, handling and laboratory costs. Types of Analyses Available Analysis I) ROUTINE MAINTENANCE CHECK Total Charge: $20.00 To determine the genera] condition of the fluid and find whether further analysis is neces sary. (one-quart sample required) Properties Tested Color and Condition Dielectric Strength Moisture ' You will be notified of the results of this test. If further testing is indicated, and you want a complete analysis, you will be sent a five-pint sample container. This sample will be used for the following series of tests: Analysis 2) COMPLETE ANALYSIS Total Charge: $50.00 (a) To determine the extent of fluid contamination, (b) earth refinement to determine what degree of restoration of electrical and insulating properties is possible, (c) check test to see how the fluid re ponded to earth treatment. a) Complete Analysis: to determine the extent of contamination Properties Tested Color and Condition Specific Gravity Refractive Index Water Free Chlorides Acidity Dielectric Strength Power Factor, Dielectric Constant, and Resistivity NEV 007566 WATER_PCB-00051027 b) Earth Refinement Response: Consists of treatment for 2.5 hours at 50-60C. with 0.1 to 0.2 percent by weight of properly conditioned Attapulgus clay and then filtration through dry filter paper. c) Analysis After Laboratory Earth Refinement: Properties Tested Refractive Index Water Free Chlorides Acidity Dielectric Strength Power Factor, Dielectric Constant, and Resistivity You will be notified of the results of this test series on your sample. Then aftei refining your entire transformer fluid fill you can check on the results by requesting the following analysis: Analysis 3) ANALYSIS AFTER EARTH REFINEMENT Total Charge: $30.00 (This charge will not apply when analyses I and 2 have already been made.) To determine whether the entire lot of the askarel fill responded to the same extent as the laboratory sample, (five-pint sample required) Properties Tested Color and Condition Refractive Index Water Free Chlorides Acidity Dielectric Strength Power Factor, Dielectric Constant, and Resistivity To arrange for the tests described above write to the following address: Paul G. Benignus Monsanto Chemical Company 800 North Lindbergh Blvd. St. Louis 66, Missouri Samples to be tested should be clearly marked for identification and sent directly to: Monsanto Chemical Company W. G. Krummrich Laboratory Monsanto, Illinois Attention: R. Kuster # 22 NEV 007569 WATER PCB-00051028 APPENDIX APPENDIX A -- Askarel Stability and Composition of Arc Formed Gas: Askarel insulation is one of the most inert, chemically-stable heat resistant, non corrosive liquids known. It will not break down, oxidize or sludge when exposed to air and high temperatures, 150C. or even somewhat higher. Arcing, however, will break down the compound to liberate some hydrogen chloride and small amounts of carbon. APPROXIMATE COMPOSITION ARC FORMED GAS FROM TRANSFORMER ASKAREL Cas carbon monoxide......................... carbon dioxide.............................. oxygen........................................... inert gases..................................... hydrogen chloride........................ (note the absence of phosgene) Amount 0.3 per cent 0.3 0.6 1.5 97.3 This arc-formed gas is non-flammable and non-combustible. These requirements must be met in accordance with the Underwriters' Laboratory for permission to use the term askarel. Mineral oil evolves combustible hydrogen and hydrocarbon gases. For all practical purposes, the amount of gas liberated from mineral oil or askarel under a given set of conditions is about 100 cubic centimeters per kilowatt-second. APPENDIX B Carbon dioxide............... Air.................................... Nitrogen.......................... Hydrogen chloride1 .... I) In absence of scavenger SOLUBILITY OF GAS IN TRANSFORMER ASKAREL Percent of Gai By Volume Corrected to: 25C. 760 mm 2sc. lore. 0C. 760 mm isc. iorc. 71% 47% -- -- 5.7 4.9 5.8 5.0 6.0 4.8 5.5 4.4 37.8 50.9 ---- 23 NEV 007570 WATER PCB-00051029 APPENDIX C APPROXIMATE VAPOR PRESSURE vi. TEMPERATURE FOR TRANSFORMER ASKAREL Temperature 'C 40 60 80 100 120 140 Inerteen PPO, 7336-9 1 mm Hg. 5 9 30 60 90 Transformer Pyranol A13B3B 0.9 mm Hg. 3.5 8.3 18 32 53 APPENDIX D EFFECT OF TEMPERATURE ON DIELECTRIC STRENGTH OF ASKAREL Temperature C. --60 --40 --20 0 20 40 60 80 Dielectric Strength 67 KV 63 57 35 50 30 48 45 APPENDIX E COMPARISON QF THE APPROXIMATE VISCOSITY IN SAYBOLT UNIVERSAL SECONDS OF TRANSFORMER ASKARELS AND MINERAL OIL Temp. C. --20 0 20 40 60 80 100 Transformer Pyranol AI3B3B 1,000 100 70 45 39 34 30 10-C Mineral Oil 1,000 ISO 85 49 40 34 30 Inerteen PPO, 7336-9 2,800 195 85 50 40 36 33 24 new 007571 WATER PCB-00051030 APPENDIX F THE DENSITY OF INERTEEN PPO nU-9 AND TRANSFORMER PYRANOL AI3B3B Approx. Density gm /cc. Tttnpcfaiare *C. 0 Inerienn PPO, 7336-9 1.374 Transformer Pyranol AI3B3B 1.577 20 1.552 1.555 40 1.529 1.332 60 1.507 1.510 80 1.485 1.488 APPENDIX G The thermal conductivity values of transformer Pyranol A13B3B at 27C. and 58C. are 26.2 and 23.8 x 10*s calories centimeters'1, degrees centrigrade'1, second'1, respectively. Or, approximately 0.06 BTU per (hr.) (sq. ft.) (F.) per foot. This same approximation applies to Inerteen PPO (7336-9). APPENDIX H Heat Capacity Over the temperature range or 25 to 125C. the specific heat of transformer askarel is close to 0.30 calories per gram per degree. APPENDIX I Coefficient of Expansion The average coefficient of expansion of transformer askarel over the temperature range 20 to 100C. is 0.0007 cc/cc/C. One gallon would increase to 1.056 gallons on heating from 20 to 100C. APPENDIX J Fire-Resistance To use the generic name "askarel," the fluids must be approved by the Underwriters' Laboratories as possessing adequate fire-resistance and freedom from forming explosive gases when arced. These liquids do not have a burn point (ASTM D92-33) (Cleveland open cup method) up to about 205C., at which temperatures they begin to boil. The significance of this is that they do not burn or support combustion under conditions encountered in transformer operation. Thus the danger of secondary explosion (or fire) is eliminated. 2$ NV 007572 WATER PCB-00051031 APPENDIX K Seals, Properties and Procurement Dow Corning Corporation, Midland, Michigan with District's at Atlanta, Boston, Chicago, Cleveland, Dallas, Los Angeles, New York City, Washington, D, C. and Toronto has available Bulletin 09-019, August 1962 entitled "Silastic Design Data". This lists the gasket fabricators throughout the country from whom the "Silastic 50" gasketing can be purchased in sheet, extrusions or molded shapes. Generally Silastic 50 sheet goods are stocked by local die cutters, hence, could be generally purchased locally. Usually, small quantities of gaskets are die cut. If larger quantities are needed, tools are made of the same type used to cut other elastomers. Where the gasket is extruded for fitting into a machined groove or between gasket stops, Dow-Coming advises use of a starved joint. This joint is then cemented using Dow Coming's Silastic 140 (clear) or their RTV 731 (white) materials, which air cure. Dow Corning points out that the local "rubber" fabricators purchase the Silastic 50 in billet form. This is worked on a roll mill in preparation for sheeting or extrusion. Then to obtain the desired physical properties the fabricator must oven cure the Silastic 50 for 24 hours at 480F. SPECIFICATIONS* Color............................................ White Specific Gravity at 77F............. 1.20 * 0.02 ASTM D676 -- Hardness, Shore A. Scale.......... 45 to 60 ASTM D412 -- Tensile Strength, psi. min.......................... 800 ASTM D412 -- Elongation, percent, min............................250 ASTM D395 -- Compression Set after 22 hours at 300F,, percent, max.............................. 30 * All physical properties measured on 0.075 inch thick samples molded 5 minutes at 240F., and oven cured 24 hours at 480F. General Electric Company, Redmond Circle, Rome, Ga., uses silicone or DuPont's Vilon wherever it is not possible or desirable to weld. For some small seals, where good matching surfaces are provided, Flexitallic stainless steel rings are used. By contacting the Engineering Services Department of General Electric Company, Redmond Circle, Rome, Ga., users of Pyranol transformers made prior to develop ment of these modern seals will obtain prompt assistance for conversion. Users of askarel transformers made by other manufacturers should contact the original transformer manufacturer, or Monsanto for assistance in converting to these modern seals. 9 NEV 00 75 73 26 WATER PCB-00051032 00**1* WATER PCB-00051033 NOTES 0 ?5 pj WATER PCB-00051034 MONSANTO FUNCTIONAL FLUIDS DIPT. BOO N. LINDBERGH BLVD. ST. LOUIS, MISSOURI MIBB The information herein regarding oblaininc optimum retulti from askarel fluids in your transformer has been accumulated by Monsanto for over SO years from the experience of makers and users of askarel transformers and it is believed will be helpful. Nothing herein shall be construed as applying to other than askarel insulation. Data and maintenance suggestions herein do not apply to the other components of the transformer. All operating and maintenance suggestions recommended by the manufacturer of the transformer should also be carefully followed. Because these maintenance directions apply only to the ukarel insulation, Monsanto disclaims any liability for damage to property or injury to persons arising from transformer operation. ' NEV 007576 Utfco Ifi U % A WATER_PCB-00051035 u u booi up, Hwart Borgni - 00 MP. Bill Maddox - NY HP* Fi 8tum - HI Munb 8# 196I MP. J. 0. Sullivan 0. 1, Linok Company Clifton# Man Jintj . Daar Mr. Sullivant Mp Howard Bargan of our co*miv haa aakad that wa lami1 your raquaat for oral toxicity information oiKAroolor produota va hava aeuta owl data on Aroolor HWIftd Aroolor 125% TMH data ara 4.15 ml/k* fop Aroolop 1242 and 3.10 mlAg for Aroolor 1254# both in rata. Z do not hava oteoni oral toxioity information on thaaa produota ainea wa do not on*Mop than aa advlaabla for uaa to food produota Tha raally algnlfleant profclaa to handling Arcelor* oonae fro* tha possibility of damtltls through rapsatad akin oontaot and tha poaalbility of apa* tamlo affaota through rapaatsd Inhalation of vapopa to axOOSSiVd OOnOSUtratlonS. . Aa you probably know# tha Ansrloan Confdranoa of Oovarnaantpl Induatrial Hyglanista haa aatabllahad a Hygisnlo Standard or MmcImm Allowable Ccnoantratlon (MAC) for aa !#it!!* working day for two of tha Aroolor produota. Thaaa data ara for Aroolor 1242# 1 Milligram par cubic meter and for Aroolor 1254# 0.5 milligram par eubio matar. Wa auggaat to milMm who handla thaaa produota that eara bo takan to avoid axtansiva axpoaura to tha mmmlmtM skin and to axoaaaiva vapor* Monsanta and lta ouilomn hivi handlad many million! of pound* of thaaa produota with m difficulty# topping thaaa almpla handling praoautionn to Bind. If wa mp ba of wy tturthar halp# plaaaa lot ua toon. Siuoortly# jr<* RBXipjk R, Basnet galily; m. d. Mdloal Dirooctor NEV 161141 WATER PCB-00051036 EXHIBIT 6D Monsanto Chemical Company St. Loots 4. Missorax ^Lu-Uk*^ ' July 25, 1956 ' Mr* Ho W. Speicher, Administrator Industrial Hygiene . Westlnghouse Electric Corporation East Pittsburgh* Pennsylvania . .. Dear Mr. Speicher: ' " ' Thank you for your letter of July -19' requesting toxicity Infor mation on several of our Aroclors 'and atmospheric sampling methods. ' I an sending under separate cover two detailed reports published by personnel at the Kettering Laboratories .entitled* "The Toxicity of tee Vapors of Aroclors 1242 and 1254." 'Tie data contained herein were condensed and presented by Dr, Tireon at the AIEA meting to Philadelphia this year. - It was published to the form presented to the June* 1956 Issue of the "AIHA Quarterly*" a copy of which I am sure you oust have. I am asMng Dr. Treon, by a copy of this letter* to send you a reprint of his publication If such Is available at the present time. ot* You will note that Dr. Treen has proposed that the hygienic stan dard for Aroclor 1242 be tentatively established at 2 milligrams per cubic meter and that the standard for 1254 be estSBXBBga^at cubic meter. I am sorry thai t we d`o not `have xL However, we have so particular '<* ^reason to expect that a sr jj.enj:..chlorinated .biphenyl offers' ^-'any greater hazard than a per cent chlorinated' biphenyl. "L/^You will note further that Dr.-Trtoo'a work discusses a modified jwJ; Willson hydrocarbon apparatus' used to the sampling of his test V atmospheres. In a limited mount of sailing to our own plants we have used the Willson equipment as shipped to us. I have en closed a description of the operating procedure prepared by one of our research groups which Is .%omewhat more detailed than that provided with the instrument ;' . You have.previously seen our complete reports on the decomposition of Prdraql when allowed to drip or flow onto-'a: heated natal Inconel surfaceThe- data to'those reports have convinced us that there la no greater'acute hazard should Pydraul accidentally contact metals at the temperatures investigated than there would be with other industrial hydraulic fluids.' I do not have any data, to .support ar.y conclusions as to what might occur If the Fydraul were to be used NPC00035799 WATER PCB-00051037 Mr* 1* . SpeIcher, Administrator -- Page 2 -- July 25# 195$ as a hydraulic fluid In aaklng cameaitm,. die.castInga. We do have a report that one planrtmanaling large quantities of molten ma^estom purposely sprayed Pydraul into the molten material primarily to aee if there would be a great deal of spattering of the maf^esium toe co^any reported to us that their testa convinced them that Pydraul could be used Whether or not they are using Pydraul, -I cannot aagr, , ' . . ... I note in rereading your letter that 1 have not answered your question relative to akin effects following Aroclor contact. ' .We recommend that repeated and prolonged tkln contact with arty or zne Arociora &e avoided/ we have patch tested, aeveraf or ' them with"Eigatlv* faults, to addition, .reported cases of |skin irritation have been surprisingly few to view of the heavy f tonnage quantities of Aroclor manufactured 'and handled to the last twenty years We believe, however, 'that care to handling and good personal hygiene is necessary to avoid irritation .* ` . .* . ' * v ./ ^ it. K /: . * -* .* As with May "'chlorinated hydrocarbons / exposure to 'sufficient quantities over a long enough period of time cbuld conceivably 'result in`chloracne.-' to this respect, however, the Aroclora are nqfcJKC^^^^cMLqMeenegsna,' such aa chlorinated naphtha- lanes--' To our knowledge, there have never oeen ahjpcasea bf chloracn* in the electrical to*astry8s use of these products If I can be of any further assistance, please let * know. ' Very truly yours. . -'* " V u * Vr ` V, -vEPWjSMB ':> ir f, Wheeler Assistant Director Medical Departaent ' * ' ' ' i.vl 'V.VvL-r'AfJt - a.*', ..'`iV'i V*i i '* " l.-' V'*:** . ^ Enclosure .A<- gift's- %:\K V, , cc Dr.1' Joseph F.*' Treon V/11 % -toe Kettering Laboratory rk v ' Mr. Pau l 0. Benlgsus ' `.-' *y 'v " Monsanto' *" ' NPC00035800 WATER PCB-00051038 -A BOG Paul Benignus-GO Oatobar m 1959 m..lift Jtre 1. Wilbur Jpalshsa> Adalnlstrator# toAntriml Hyglsnt lloatrla Corporation ast Pittsburgh, faimsylvaala Bsar VUhuri Viaak you for yew lottar of 0tobr 21 Inquiring about the aft uaa of trlshlorodlphsnyl and a nlxtura of 4<p fcrtMr- bsnasoa and 60)1 . Vt narkst trlahlorodlshanyl /^JItIqc 1242") Tha sonblna- tlan of haxaahlarodlpiMNagrl trltlitowottonwant Is known sonblnatlan la our fha ptqralaal and ahaadaal proportion of tha Aroalors osntlsnsd aura Shown on tha tabla on pagoa % and 5 of tha onoloaad Areolar bullstln# maloaad alao la a reprint IndlaatlM tha results of shrenls toxleity atudlas with ArealmnQMtm and ia$4, tha following acaaaata answsrlng your quaatlons oarlally are IumI m lnforaatlsn ssntalnsd in thasa bullstlna. X toallava paroiongad and repaatad akin aontaat with any of tha Aroalora should ha avoids* for two reasons, In tha r&rat plasa, tha lata shlarlnatsd product* art llfulda and are mmI lant solvanta f? oils and fats in tha udn m wU as dhir organla aatarlsla, tasondlpf i% it poaslbls that ^ttd m repaatad aSdR omlMl sould land to shlsrasaa* Z lorn of only lw sasali share auah agpsrlansa has drtolopod during tha loot history of production and uaa of tha Amlon to ona saaa* an Arealsr was ball* mad m a htl ttmifir asdlua In a 9j%%m that aUMii vapor* to oaaapa whan tha aatar&al was haatad ta 600% favors1 norteon davalopod "blasbhoada" ahloh wore found fey ft Industrial physlslan but whleh In his wr4* ware sa in* algnlflaant that tbs mu ware not imm of than dot would a ganoful pmMMXimmw mtis^ thin, Shis Indlaatss to na* howavar. 1 DEPOSITION II EXHIBIT 1 NEV 006347 WATER PCB-00051039 Up. B. Wilbur fpalohar--fag 2~October 83f 1959 that sufficient exposure, *i#ther by inhalation of vapor* or kin oontaot# can result In ohloraen# which 1 think we oust assume could be an indication of norc serious systemic Injury if the mpmum waa allowed to oontinuc. A second ms of nUd ohloraon about which we have any kmwlAdgt resulted from tiortanen dipping their hands In the liquid Aroelor as if it were mineral oil or vegetable oil. Zn addition, their clothing sooner or later became Impregnated with the material and thus exposure was magnified. Tcu ak#d at what tenperature local exhaust ventilation should be provided. Although the distillation range for Aroelor 1242 ia 325-360C. and 385-420<>C. for Aroelor 1260, I feel that good praotiee diotatea that looal exhaust vantilatlon be provided when any of the Aroelora are heated above 1507. in open tanka or in any ayetea* where the material la not in a completely aneloaed system (vapor-proof tanka, kettles, pumps, piping, ete,), This may be ultra conservative because aa the distlllatlon ranges and vapor pressure curves (page 12 of the Aroelor bulletin) indicate, the losa of vapor* at 1507. should not be significant except in any work area where general ventilation or air ohanges do not exist. Your next question related again to possible skin and systemic effects and I believe it is answered above. In connection with the 40^ trichlorobenzene-6o Aroelor I860 combination, 1 believe the thoughts expressed above also apply. X understand that the trichlorobenzene which Is used is a mixture of the 1,2,3-# 1,2,4-, and 1,3*5-isomers which will begin to distill at 205C* Again, I believe this indicates a low vapor pressure for the solvent st room temperatures. The only reference m have to triohlorobensena toxiolty is con tained in the Publio Health Service Publication No. 414 entitled "the Halogenated Tootloity and Potential Dangers" by Dr. W. 7. von Oettingen, 0.8. Oovernment Printing Office, 1955 (paxes 297-S98). fir. yon Oattlngen refer* to tens wo* done in 1937 <Aih indicated that the trlehlorobenaene was less toocie than mmo or dishlorobensene. in my opinion, a reasonable MAC for tliia material would be 100 pavta per million. The anoloaad publication on tha toxicity of Aroelor 1242 and 1254 suggests an MAC for 1242 of 2 milligrams per cubic meter which is twice that rtoeiiMended by the AC01H for a chlorinated di phenyl of unctatsd chlorine content to the ease of 1254, the publication suggests that the MAC of 1 milligram per cubic meter "ree amended tentatively for safe indutrial practice by the Amarlean Confaranaa of Oovarmantal Industrial Hygienists* is reasonable, to the ether hand, reference to Henry Aayth's Cummlnsa Namsrlal |4tw of I956 in which he discussed the Mai* for the then xUstlm* -hyiitnie atandards" indleat#* that 006348 WATER PCB-00051040 Hr. Vilbar feolahor--ft 3--0tb#r 83# W9 . that NlkOs of 1 a^faua* for Aroolor 1248 and 0*3 a^um* far Aroalor X894 aro boto roallatlo* Xa tho abaoaao of aiqr aturonla toalolty data on Imiw I860* aa auggaat an NM) 9t 0*5 Ba/tua, tho mm m 1a tho aaaa of 1834 X tow toiaa la oao plant ahora thaao aatorlala war uaod for #apItr aM tranaforaara* tho aara and luMUng and tha prmt^lma of oxbauat vontllatlon mm not in aooordanoo with tho thoughts upftiMd abovo* Tha only roportod dlfflaultF m aona mU4 ayo lirltatlan vban Imprecation aablaata iten tho itaaa vara tjoatod to 110-ltDC. roloaaod of trihlvo* baaaano uni tho Aroolor into tho vnan tho tabtooi ten loaod* Xtt ay Bind# Nb aablnata iNuU ho vontUabod to tte voooro ratbor than Um than to to nlnati into tho X tow boon told that roar aonpoaor to* had aona 80-83 raara1 nu.uo's-U/u-uo with tha produota dlaouaaod atow* Xt wa iuuiiMI Uul Rr Jhaaa 1 Ford* msuiiif C tranafonaar aanuftaturlns onalnotrint at jots1 Bmrm Fiant would to A i >00000 of laferaa%lm rocaxnlna ooparlonoo with Saortoon FFO. dlallarly# Mr# l, X ttorburar of rour BlooBlngton Indiana Float to* boon *alAi#4 vith tho uao of Awiw 1248 Fovhapa jm hava alraoAr dlaauaaod potential m9mf with thaao gantloMn if m, X *M to lateraatod In laaminc of tholr paantloal ox- ,,;;j0 *lth feu.-; produatO. X Mute to {':: you to FAttaburgh naxt dlnoavaly* With iNlNUNI 8 Murnr F ttwolar Militant BdraOtOT Ntelaal. Popartnon* NV 006349 WATER PCB-00051041 bcci Paul Benlgnus April 26, 1966 Mr Alvin V. Crow Qumrierman Maintenance Public Works Department U* S* Naval Station Kodiak* Alaska Dear Mr Crow: Your letter of April 15th ha* been referred to me for repljf. t I have enclosed a booklet which desorites fire resistant transformer fluids which have the generic name "Askarel." You will note on page 2 and page 3 of the enclosed Askarel Qulde that there are several commercial or trademark types of formulations* sane of which are described in tables 1 and 2. Chemically these transformer fluids are mixtures of chlorinated diphenyl and trichloro anchor tetrachlorobenaene. The history of the manufacturing* handling and use of these products dates back approximately 30 years* In that time there have been no caaea of serious illness or toxic effects when simple precautions to avoid exposures have been followed. In the case of chlorinated diphenyls* a Hygienic Quids has been published by the American Industrial Hygiene Association for the materiala containing 420 and 540 chlorine* The diphenyl in Askarel is diphenyl chlorinated to 600. The toxicity characteristics then are believed to be similar to the 5^0 chlorinated material* The hawd {m differentiated from toxicity) la less in handling iheTSDStTSaterial since it is less volatile than the materials with lower degree! of chlorination* The vapors from transformer Askarel are somewhat toxic and should not be breathed continuously over a prolonged period of time* With the fluid at rocs temperature m would expect that there would be some odor of the fluid* The level or concentration which Is barely detectable by smell should not be hasardous. to the other Mod* if the fluid Is heated and vapors which are liberated sre allowed to aocumulate in an (i DEPOSITION I EXHIBIT 1 sn I NEV 161229 WATER PCB-00051042 HP* MvJj V. CrflW April M0 1966 m* t unventlisted rom or mm# fell concentration oouM became significant. In pn:1| paapla an detect * emmlntion in the amount of 0.5 to 1.0 g per oublo meter of air which Is regarded aa the aafb vortooi limit for an 8-hour daily exposur* (5 days a week# week in uul week out). fnnalonwr Aakarel accidentally spilled m tha skin d@n not present an aoute toocloity tmsard nor will it mum mrloua irritation Zt should be raovtd from the MOn by washing with soup and water, however, because repeated and prolonged exposure may lead to drying and chapping of ths skill baoauaa of tha "solvont motion" of ths fluid -- which Bight bo compared to the drying of the skin from using paint rmtr or many othor solvents in s caroloss fashion. Vapors in high concentration* when Um fluid is hsatad will eausa aya irritation. It is pointed out on page 5 of the onolossd Askarel Ouite that typical opthalaio solutiona or ointaenta for relieving pain in tha eyee may ha uaad aftar flushing tha ayaa with large amounts -of water. Long rang# seoumulstlva affoots from exposure to Asksral fluids mild not te mooted unless workmen were exposed to high lavals of vapors s number of hours m day, day in and day out or allowed the material to remain on tha skin for prolonged period* of tins and at tmqmnt and rapaatad intervals. Excessive vapor lnhallatlon or akin eentaat cm lead to an effect on tha liver aa Is the ease with many chlorinafeiid hydrocarbon*. Us hmv* nsver heard of such effects in wovkmm installing# repairing or servicing trAnsforneWj, however. If exhaust ventilation oannot ba provided to ranova tha vapors ralaasad by leaks, tha wericmi) should ba provided with respiratory protection equipment if repairs and servicing are required in an araa whara tha vapors are Irritating fete eyee and nose or throat. If I can ba of any further aaaiatanoa# plassa do not haaitata to lat m toon Very truly yours# Re Bnet Kelly, M.D. ftedieal Director Enel. Askarel booklet Hygienic Guide "Chlorodiphenyls NEV 161230 WATER PCB-00051043 ^v. ru. tur o o HYGIENIC GUIDE SERIES Chlorodiphenyls (Containing 42% and 54% Chlorine) o /W\ O o o o o o (x 4 y - 3 or 5) Cly Significant Physical Propartial1 The chlorodiphenyl* are light straw-colored mobile (42r* chlorinated! and vucoui (b4Te chlorinated) liquid* vuth typical chlorinated aromatic odor*. These compound* are chlorinated to specific weight* of chlorine. Chlorodiphenyl (42%) contain* 42.0 = 0.5 chlorine, an amount corresponding to three chlorine atoms in unassisned position*. Chlorodiphenyl (54<"r i contain* 54.3 % chlorine eorresponding to five chlorine atoms in unassigned poiitions. Both compounds* are insoluble in water, but soluble in bentene, kerosene, acetone, amyl alcohol, ether anc_ chloroform. - Chlorodiphenyl (427c) Chlorodiphenyl (54%) Molecular weight: 247.53 126.45 r Flash point (Cleveland O. C.): Distillation range: 176 -180 C (319' 356* F) 325*-366*C None ity.m'c. Sperific gravity: Vapor pressure: 1.381-1.392 (25V15.3*C) 1.495.1.505 (65*/I5.5'C) 0*C 0.001 tnm 0.00006 tnm 25*C 0.006 mm (est) 0.00054 mm {eat / 150*C 4,3 nm 1.4 nun 200" C 29.0 mm 9.0 mm At 25*C and 760 mm Hg: Saturated air contains 0.080 mg/liter 0.009 mg/liter ! mg/liter = 1 ppm = 98.8 ppm 0.010 mg/liter 74.9 ppm 0.013 mg/liter 1. Hygianic Standards A. Recommended maximal atmospheric concentrations (8 hours): One rnilligram chlorrtdiphcnyl (42fr) per cubic meter of air and 0.5 milligram chlorodiphenv) (54`r I per cubic neter of air.1 This is based on the results of The CarasitK* wiihfii M sckiwwMc* tfes pf^parati* W (La Mdicat information treti** ( tks Guide be tha larfutltisl H>(ko* sad Cliiie* Tmicotoer Qmitt al I. M. A., sad to ockuaolodn W tb *v inane* of Efaer nPu. idWc.h**Wr and Jack T. Garrett in the ( tha chronic animal inhalation studies.1 R. Short exposure tolerance: Ten mg of a diphenyl of unspecified chlorine content per cubic meter of air has been reported as unbearably irritating.4 C. Atmospheric concentration immedi ately hazardous to life: Not known for man. irritation of the eyes, nose and throat a; levels which have not caused acute illness preclude the likeli hood of voluntary exposure to immedi ately hazardous concenu ations. r3nA -- ADM 005640 WATER PCB-00051044 Jinuary.pfbruary, 1965 II. Toxic Properties . A. Inhalation: Experiment! with ehloro- dipltenvl (42*6 chlorine) were run at concentrations of 8.6 fit;/liter and at . 6.83 ftg/litcr of air. Cats. mice, rabbit! and rati were unarmed by the higher level while guinea pig! showed poor growth after lcventeen 7-hour/day ex posures over 24 days. Eightv-four 7hour/day exposures at the lower con centration had essentially no effect on similar species of animals.* In the cate of chlorodiphenyl (54% chlorine) eightv-three 7-hour/day ex posures over 121 days to a concentra tion of 5.4 fig/liter resulted in injury to liver cells and increased liver weights in rats. At a concentration of 1.5 fig/liter for one hundred and fifty 7-hour/day exposures over 213 days, the rats showed distinct microscopic changes in the liver.* The literature contains many refer ences to the potential toxic effects of chlorinated diphenyls in man and ani mals. The early work included investi gations of chlorinated naphthalenes, chlorinated diphenyls, chlorinated diphenyl oxide and various mixtures of these. An early report indicated serious toxic effects from chlorodiphenyl chlori nated to the extent of 63%.9 A later report by the principal author properly identified the earlier sample as a mix ture of chlorinated diphenyl and chlori nated diphenyl benzene.4 However, only a few authors of subsequent papers, bul letins or textbooks have noted this cor rection and the original data are cited repeatedly as relating to chlorinated diphenyl alone. B. Skin contact: Both compounds are readily absorbed through the clipped, intact skin of rabbits. The minimum lethal dose when the undiluted mate rials were applied to the covered clipped, intact skin of rabbits for 24 hours was approximately 1.0 gm/kg for the 42% chlorinated and 1J gm/kg for the 54% chlorinated.' Local .xtion on the skin is similar to that of common organic solvents where contact leads to removal of natural fats and oils with subsequent drying and cracking of the skin. ' Human cases of clUoracne have not been reported from the use of these two specific ch orodiphenyls. The potential undoubtedly exists because of cases which were reported from the use of chlorodiphenyl with a higher chlorine content and from mixtures with other chlorinated aromatic compounds.9 *-* C. Eve contact: The liquid products and their vapors are moderately irritating to eye tissues. ' D. Ingestion: The acute oral toxicities of the undiluted compounds arc not gn-at as evidenced by oral LDw`s in rats of approximately 8.65 ttm (7.61 to 9.78 fro) per kilogram for the 42% chlori nated and 11.9 gm (10.48 to 13.45 gm' per kilogram for the 54% chlorinated.' Central atrophy of the Uver appears to be the chief toxic effect III. Industrial Hygiene Practice A. Industrial uses: The chlorodiphenvls are used as dielectrics for condensers.* capacitors and transforuiers, plasticizers:, in synthetic resins, in emulsion adhes- ives, as nonflammable hydraulic fluids and as transfer media. <- B. Evaluation or exposures: ' 1. Air sampling and analysir: a. Direct field methods: None b. Laboratory methods: . (1) Collect in secondary butyl alcohol in fritted bubbler or two large impingers in series; concentrate sample and complete analysis by one of various methods for chlo rinated hydrocarbons.4 (2) Sample air through com bustion furnace, collect chloride ion from decom posed chlorodiphenyl in suitable alkaline solution and determine chloride ion con centration.9 C. Hazards and their recommended control: 1. Inhalation: Absorption is chiefly by initiation. Concentrations in the workroom atmosphere should be maintained below the recommended levels. Where the chlorinated diphenyls are used at room tempera- ( C C C c o o ADM 00 5 8A 1 WATER_PCB-00051045 o o o o o o o o o January-Fcbruary, 1965 . turn, the hazard of inhalation is elevated temperatures, the pattern considered slight or absent. When should be moved from exposure and these . materials are subjected to kept at rest until seen by a physician. elevated temperatures, the process Oxygen should be administered if either should be completely enclosed breathing is difficult. or other adequate mechanical ex haust ventilation must be provided to reduce concentrations to safe Eyes contaminated with chlorodiphenyl should be irrigated with water for at least 15 minutes and the patient levels. In heat transfer media appli should be seen by a physician. Depend cations, the system must be designed ing on the amount of inflammation and and constructed so that it is leak proof. Special gasket materials and E seals are available to present je. The reservoir tank should pain present, drugs like Cortisporin1 ointment and topical Pontocainc1* ntav be indicated. be airtight except for a vent to theB. Special procedures: Persons who are outdoors. In tire event of spills or regularly or rr|>eaicdly exposed to chlo leaks of hot fluids, use chemical rodiphenyls should be examined periodi cartridge respirators or eas masks cally to detect early evidence of skin approved by the U. S. Bureau of irritation and /'or liver damage. Persons Mines for protection against organic with known liver disease should not be vapors. These will provide good exposed to repeated contact with the protection up to the concentrations chlorodiphenyls. shown on the approval labels and the odor will give ample warning if V. References it comes through the device. 1. Monsanto Company, Organic Chemi 2. Skin contact: Operations and handl ing procedures should be such as to avoid the possibility of prolonged or repeated skin contact. Contaminated clothing must be laundered before reuse. 3. Eye contact: Eye protection should be used where there is a possibility* of liquid splashes. 4. Ingestion: Ingestion of these mate rials is not a problem in industry. cals Division: Tech. Bulletin # PL-306, Aroctor Plasticizers (Dec. 1960). ' 2. American Conference of Governmental Industrial Hygienists: Threshold Limit Values for 1964. .4.\f,4 .4rc/t. Environ. Health 9: 545 (196+>. 3. Treon, J. F., F. P. Cleveland. J. Cappel, and R. W. Atchley: The Toxicity of the Vapors of Aroclor 1242 and Aroclor 1254. Amer. lnd. Hvg. Assoc. Quart. 17: 204 (1956^. ' 4. Elkins, H. B.: The Chemistry of Indus 5. Fire and explosion: The chlorodi- trial Toxicology. John Wilev and Sons, phenyls are fire-resistant or essenti Inc., New York (1959\ ` ally nonflammable liquids. When 5. Drinker. C. K., M. F. Warren, and G. exposed to flame or hot surfaces A. Bennet: The Problem of Possible they may decompose to form CO, Systemic Effects from Certain Chlori GOg, HC1, phenolic and aldehydes nated Hydrocarbons. /. lnd. Hvg. Tox depending on the temperature, avail icol. 19:283 (19371. ' ability of oxygen, area of the heated 6. Drinker, C. K.: Further Observations surface, rate of application of the on the Possible Systemic Toxicity of liquid to the surface and other Certain of the Chlorinated Hydrocar variables. bons. J. Ind. Hyg. Toxicol. 21: 155 IV. Medical Information (1939). _ 7. Wheeler, E. P.: Personal Communica A. Emergency treatment'. Skin surfaces tion, Monsanto Company, St. I^suis, exposed to chlorodiphenyls should be Missouri 63166. thoroughly washed with soap and water 8. Greenburg, L., M. R. Mayen, and A. at once. If clothing has been contami R. Smith: The Systemic Effects Result nated it should be removed promptly. ing from Exposure to Certain Chlori If exposure to a high vapor concen nated Hydrocarbons. /. lnd. Hyg. tration occurs, as in the case of spills at Toxicol. 21: 29 (1939). . o 6 WATER_PCB-00051046 HYGIENIC GUIDES COMMITTEE C. P. Caapcster, Chmrmm N. E. Bolton' E. E. Cam mu. J. W. Clayton H. B. Elkins P. D. Halley Mau Hrre J. A. Houghton D. R. McFcc J. M. Mc.Veeszy, J*. J. E. Peteeson J. B. OusM.virsKi t A. PrTTSEI U. C. PoEEANI i- L. Raleick W. L. Sutton R- C. Wands 0. L. Wilson Hygienic Guide sheet* may be obtained from the amksica.v indystsial hygiene asiocia- tion. 14125 Prevost. Detroit 27. Michigan, at 25 cents each for two-page reprint*: JO cents each for four-page reprints. All orders for less than 12,00 must be prepaid. Discount of 2VA on orders of five or more Guides: 4Ki discount on orders of 100 or more Guides. Special looseleaf binders for the Guides may also be ordered from the Association office for $1.25 each. C O o o a n m nntiui WATER_PCB-00051047 - fV ** ) Monsanto Moniinla C<n,,ny $00 N. flti eyMvtrtf SUtttli, MUtontl (SISS Fhoa$! OUt $94-IOOO TOXICITY AND SAFE HANDLINQ OP ASKAREL On the basis of animal toxicity studies, the Askarels may be considered only slightly toxic from the stand point of accidental ingestion or a single accidental massive skin exposure. Similarly, single exposures to high concentrations of vapors (when heated suffi ciently to volatilize) or high concentrations of decom position products (if the fluid is accidentally discharged into the fire chamber) are not serious hazards because the irritating character of such concentrations preclude voluntary exposure. Repeated or prolonged skin exposure should be avoided since the Askarel fluids act as solvents for fats and oils of the skin. Removal of these natural, protective barriers can lead to drying and chapping such as oocurs with exposures to paint thlnners. More important, the fluid may be absorbed if it is allowed to remain on the unbroken skin. For these reasons, we recommend that the skin be washed with soap and water if there is con tact. A skin burn resulting from accidental contact with hot fluid should be treated in the normal manner for any thermal burn due to hot oils. Because of low vapor pressure, there is no significant vapor Inhalation hazard when an Askarel fluid is at room temperature. For example, there ia no vapor exposure problem while transferring the fluid from its shipping container to the using equipment. On the other hand, -the vapors emitted by Askarels heated to elevated tem peratures are Injurious on prolonged or repeated expo sure. The "Threshold Limit Value" or atmospheric vapor concentration which cannot be safely exceeded (on a daily basis) la 0.5 - 1.0 milligrams of Askarel vapor per cublo meter of air in the workroom. March 4, 1971 R. Brunet Kelly, M. D. Medical Director WATER_PCB-00051048 Monsanto EUROPE 8.A. PROM : tMAMk 4 LOCATION* ^ Brussels, Belgium DATE ; February 22, 1967 SUBJECT : RFFERENCE : DW TO : Dr. R. Emmet Kelly St. Louis CC : J.R. Buchanan, St Louis J.E. Filer, Brussels D.V. Hardy, MCL Eugene Wilde, St Louis Dear Dr. Kelly, I should like to refer to your letter dated the 10th of February and our telephone discussion of yesterday's date. I enclose a copy of Sttren Jensen's original paper' which in fact was presented in English - Dr. Jensen apologises for the typing etc. but this copy is taken from his original paper which has not yet been re-typed and tidied up. I asked our agent in Sweden to dig out the various pieces of information that you required and I attach a copy of his reply dated February 17th which I think fully covers the point raised in your letter. If there areany small points outstanding, please let me know and I will try to get you further information. I am sending the only copy of Mr. Jensen's paper to you and therefore if any of the other recipients of this letter needs to have access, they can take a copy from yourself. I would however emphasize the post script on page 3 of Ola Palm's letter in which he states Mr. Jensen has consented to send us the full copy of his paper on the understanding that this is used only internally within the Monsanto organization. 1 DEPOSITION | EXHIBIT | 3a 1 NEV 023647 M-3 WATER PCB-00051049 Q f c/Ua. ^,r * .'*1 :// i . i*' Mr Chatmanf XioAlt* And gontle(nen, * In honor to our Brlttieh fceot X will try to hold thlo lecture in Kngliob. ' ii tho tltlo of thlo lecture stateo, X on today going to toll about \lN\ tho dloooTory of sobo hitherto unobserved ohlorloatod hydrocarbons having up to eight ohlorlno In the Molooulo and found In residue ena- lyolo. She ehonloal none of polychlorinated blfonyla ( In tho following colled BOB), So got familiar with PCS X will ot&rt with the choclotry and .tozicologi. Ohonlatry Sh 5.U t ^ t i *" ti/ 7V--6- j `V / Sho main ohoraotorietlo of PCB le 1. Shefr Very high stability. i.o on example they can be boiled with nltrln aold without being destroyed. 2. They are hardly netabolleed In living organism. 3. If oro than 4 ohlorlno are pro^sent they are non Inflomablo. It le elear that those three oharaoterlatlos does It easy to understand that when they havo entered the living organism, the will have a low persistence . But it Is difficult to explain how they find their way Into tho living organics. One thing eeens to be dear, they don't oomo from agricultural uoa, but froa a teohnical one and Boat prohahlo It domoe to the nature via wuatoa that are tried to bo burnt up, beoauoe then wo have thou at onoo In tho air, booauao of their non lnflamabillty. .goxloolod A NEV 106549 The PCB woro lntroduood In 1929 and m early 1936 Jones and Aldon j reported that 23 out of 24 non employed In nanufacturlng of PCB oufferod froa aa acno fora oraptlon of tho akin, lone did not nppoar until 6 to 8 months after tho notarial was first uood. In 1937 Drinker roportod that rate exposed to chlorlnatod biphenyls In concentration of approxlaatoly 1 mg/a^ for 16 hours a day for 6 wooke ohov/dd damage of tho livor. After that time tho allowed ooneontratlon of PCB In air lo 0,5 ag/t^. , (Por PDt tho sooe value la 0.9 - 1 mg/n?), Sho name authors finished ' tholr experiments In 1938, and related that thooo oonpounde have on Injourloua offoot, nanlfoetod solely In tho liver. Chlorlnatod bipohnylc! ^ appeared to bo tho Boot lnjourlous chlorinated oompounde of all tested. ( * WATER PCB-00051050 o o 2. \ t Orenburg, Mayor and Smith 1939 roportod that PCB and polychlorinated oaphtolonoa are blamed for the death of three young workers,. and that" prognant women and poraona who have at any time had any liver diocaooo aro particularly suspeotible. ' ftdol, Haller and Benton gave 1942 animal* PCB Including odminiotrotion ! j j I by inhalation, ingootlon and akin aboorbtlon. Jlietologioal examination Of tho viacora ahowed important toxic effect only in tbe skin and llvor, and tbe dogenoratlon effect* in the liver aro eeaentially the ooae what- ; j ever wee the method for the administration. Paribok (1955/ found as an occupational poison in the eleotrioal industry, mixed tetra and ponta : J cbloroblphenyl oausos folliculitis, comedo, pyodonia and other skin affootlona, and that it* principal toxio offset is fatty degeneration of tbs liver, Miller (1944) injeoted 69 mg PCB (4 and 5 chlorine) suboontancouely in I j J 32 gulnoa pigs. Eight to ton days after Ingootlon, fat dropleta wero noted in the liver eelle, and after 16 dayo they were present in moderate ! j or very large numbers. Babbits and rats were also tested in this invootl- | gation, as wall as the PCB wae adminlatated both contlnouely, oubcontla- : ouely or ingested In the food. In "the feeding experiment 8 guinea pigs received 2 doses of 69 mg of tho chlorinated biphenyl 1 week apart. Death ocourred in 11 to 29 days. Finally Mo Baughlln 1964 reported a method to toot tho chemical toxicity and teratogonio offset by injection into the yolk sac of fertile egge j prior to incubation. PCB wae found between the eight compounds among 100 tested having the highest order of toxicity. Ho hatch was found at a level of 25 mg po egg. At a level of 10 mg per egg, one chick hatched | J j out of 20 injected egge, but died 2 days later. Some embryos which wore j examined after they died, ohowed weak deformities (ofton a short upper brak): and growth retardation. Dead aeetate resulted as an example in no hatch < t a lavtl of 1 ag per egg. Autopsy of the dead byes have showed exton . j lve brain damage. Mercurio chloride showed no hatch even at a level of ; 0,5 mg per egg. As the analytical ohomiatry is a pronounced service science I have boon in contact with many scientists from other fields during the work with residue analysis, and I have always found this contact very stimulating for my own work. This co-operation often demand* that we are talking the same scientific language. Because of this need I will today try to give a lecture in low level analytical ohomiotry for biologioto, illustrated by tho reoldue analyolo of polychlorinated biphenyls. Sht lecture will be divided in the following throe sub-divisions: ------- --------- ------- NEV 106550 WATER PCB-00051051 o o3 1. Chemietry of JOB and their toxicology. 2. Analytical Methods for residue analysis and proof of atructuroo. 3* Behaviour of tCB in nature, dlfferenciee in metabolioing rato of the POB components, potenoatlon in an ecologleal oeria, conoentratlon lerels and exonplee of samples whieh have been provod to oon- . tain BCB. A residue analysis can be dlvldod ini ' 1 Extraction of the pesticides from the biological material, * followed by a careful oleanlng-up to take away lnterforring aubetanoee, moat often fata. t 2 Identification analyels by mean of gas chromatography. Thln- ,, layer chromatography and masa spectrometry. 3. Quantitative anolyeia. , ' . At on ecological laboratory in fiikamuedet in Btoekholm 1-2 g of a somplo ie out out of the biological material and transferred into a welgbod and carefully cleaned tost tube, and stored at -20 until analysis. Smaller samples hav# been used, min. 5 mg of body fat, and with dry materials such as hair, feathsrs, pin needles 100 mg are euffioient to reach the desired 10 nj/g level in residue analysis. In oases of water proofs 1 1. is used for reaching the 10 pg/g. loyal. B.l(homog) In order to facilitate complete extraction of the fatty materials from the biological sample, the doulbe amount of finely powdered anhydrous magnesium sulpbatt is added to the sampling tube, and the whole is honogenieed with an insertable homogeniser. The resulting powder is transferred into a apooial Soxhlat extractor. After 4 hours of extraction the colvont is evaporated, leaving the fat in a small weighed test tube at the bottom Sox,-tube) of the extractor. This fat la dissolved in methylene chloride in such a .way that 100 ul (o,1 ml) contain 20 mg of fat. She 100 ul solution is now transferred to a little object glace, 3x7 cm, covered with a sllioagel layer 1 mm thick, in order to fora a line 0,7 cm from one end of the slide. Inserting this thin-layer plate into a vessel the bottom of which is eovered by a few mm of methylene chloride, tho advent will be sucked up in the dry layer of eillcagel, and at least reach the upper end of the plate. She fact is that the fat bee a greater affinity to the powder on the plate than the chlorinated hydrocarbon have. - and we get a separation. She fat being more polar than tho chlorinated hydrocarbon will never go longor than 2 cm before thi NEV 106551 WATER PCB-00051052 I o o 4I v BwraiotJ tuba 5 6 go solvent roachoa the upper part of the gloss. Tho front of the fat eppoara %ulto vlolble against a lamp, and with tho mid of a rasor blade tho sone above the fat la transferred to the elution tuba end tha chlorinated blooldoe absorbed on the ponder oan non be luted by ono ml of ether. The concentration la sufficient for detcotioiv of the chlorinated hydrocarbons down to the 10*^ g level. Tho next step la tho analytical procedure cencerne the separatin'.: of tii* different chlorlnatod hydrooarbono that tha one.pi e */ ,va-m: t. . nattor of foctf this ie a troublecone task. It le easy to tatimfsc vhtt la not prosent, but more difficult to aay exactly one la present. Tt cuffor from the negative demonstration, as will be ohown later. At first a fen words about tho separation of tho oonpononte proaont In the aaapla and their visualisation. Tho separation lo accomplished by Man of a gas chromatograph fitted to a detector that transfers Its Inpulse to a recorder. Tho syoten Is shortly desoribodi A spirally fernod glass tube with an Innor diameter of 2 na and about 2 n In length is filled up by a support, covered with an thin layer of tn oil. The tube la heated In the chromatograph to about TOO0. Through tho tube a stream of nitrogen eontlnouely follows. When about 10 ul (1/100 of 1 Bl) of the purified sample la Injected Into tha tube, the components of the sample will be evaporlsed and go forward through the column with the gas stream. As the constituents havs different affinity to the column filling thoy dll pass the column with different speed and it will toko different tine for then to roach tho detoctor at tho other end of the glass tube. If the temperature and the nitrogen flow are held constant this time, the retontlon time, has a spoclflcvalue for a certain compound. Shis is true, but unfortunately It is also a fact that two components oca have the samo retention time. This Is one of the bigger problems In gas ohromatographlo analysis of unknown samples, as will soon be obvious. ' To make It possible to ostlmato the retontlon time It Is neoeseary to Visualise the chlorinated hydrocarbons. Tor that purpose Bore or loss peciflo detectors are used. Tho detector most often usod in poetlcldo analysis Is the so eailed elootron capture detector, which oan detect down to ono ploogram ( 10~^2 g of llndan). Unfortunately this detector Is not specific for chlorine, bu glveo answer aloo for oxygonoontalnlng compounda. The roeponee here le mvttfy lowor but can be counterbalanced if tho concen tration of tho oxygon containing Is much higher. The principle for tho eleotron capture detector lb shortly: At the end of tho gee chromatographic tube le plaood a llttlo tubo con taining a foil made of titanium tritldo. This le ap-rodiant. The p- NEV 106552 WATER PCB-00051053 o o5 particles ar# Mooting with the nitrogen molecules coming iron the column, then we get Hj -- " H^. Over the dctoctor m have tension of 90 volt and by aeon of the electrons wo will got a constant electrical eurront over the detector. This standing current, le transferred to a one-mY recordor ae a oonotont baseline, then now a chlorinated hydrocarbon leaves the column this compound hao a high affinity to the eloetrono and this aeane that the amount of elootrons will diminish, and they will diminish proportionally to the amount of ohlorine. Tho electrical current will also diminish and this is noted as a peak on the recorder. Tho area of the peak will be proportional to the amount of substance in the aample. By aean of a standard injection it ie now possible to compare the reten- , tion time and the area of an unknown component with the retention tine and area of the known standard. As said before this detector is not speci fic for ohlrine but anyhow vary useful, because of its high sensitivity. The system described has, as we have seen, two disadvantages: t. Two different compounds oan have the some retention time and bo detected ae one peak. 2, A regietrated peak does not need to be chlorinated , becauoo tho detector is not speclfio. If the sample le injected In two different columns with different chemical properties we have increased the chance for a good separation. If two compounda have the same retention time on one column they may not have it on another. When a result seems doubtful, - if the compound being responsible for a certain peak contains chlorine or not - it is possible to concentrate the sample and analyse it on a lesa aenoltlve detector such as the nlcroclouaetrle one, which is specific for ohlorine. The compound la burned In a furnace and teh generated chlorine titrated directly. As is seen froa the two lest aentloned possibilities it is anyhow possible .to gat a rather high degrse of certainty in residue analysis, but it is rather tlae-consumelng work.When using this aethod just described, we very Often found that aany chromatograms from residue analysis of most oarefully purified samples still contain a large number of peaks. liapy of these have retention times that do not agree with any known chlorinated pestlcldea, or their metabolites, Thle chromatogram con serve ae on example. It was obtained by residue analysis of a sea-eagle found dead in the archipelago of Stockholm. In the range of the known peaks, there are eo many unidentified that there also must be an obvious risk of the .. known peaks to be covered by unknown nor.. If this remark lo found true, the reported results of many previous quan- NEV 106553 WATER PCB-00051054 6 oo titablve analysis must be brought into question. In the procent investi gation it le shown that moot of the unknown peak of chromatograms at residue analysis of chlorinated peotloldoo are due to polychlorinated biphenyls. { will ehow a chromatogram of human fat analysed on a so colled SP 96 column| the moat often used type in pesticide analyses. Early retention times wore in agreomont with DDE. DPTop and PPTpp. Hoxt elide ohowo tho same sample analysed on a QK-1 column. Now the former 2 PCI peoko havo ' divided into 4 peak#, and two of them are silll in agreement with PP'jpp and op.t the two new were unknown. logically, these unknown eooponents were at first thought to be metabolites of the insecticides. Against that spoke that nelgther treatment nor . concentrated sulfuric sold in other. This treatment made It rather euro that the compounds did not contain osygen. In Sweden residues of organic sox eury have been investigated rather intensively in the Swedish fauna. As these compounds give very high responses to the electron capture detec tor it woe also investigated if the unknown peoko could have a morcurio origin. It was found that tho water-ecological series.had .high residues of both meroury (Weotermark.Johnela) and the unknown ones, when the oaae indivi duals were analysed. Anyhow, the pheasant suffering moot from mercury poisoning only contained low levels of electron capturing compounde and these belonged to the normal inaectieides. Therefore the unknown could hardly be mercu rials or metabolites of then. As the eagle aample giving the chromatogram shorn in fig. 10. could be estimated to contain KPT and DEE up to 13 g/kg in extractable fat, the amount of unknown compounds also were suggested to be in the seme range, and tehn sufficiently high to do a run on the combined gas chromatograph mass spectrometer. If this oould be done successfully it would be possible ' to get very important informations about the chemical nature of the unknown, for ex. the molekular weight numbers of chlorine etc. Thia method is up to now the method giving the highest degree of certainty in the low level analytical chemistry, amounta of 100 ng substance being enough. As this method for identification of totally unknown residues surely will be very important in the future (when f,ex. a biologist has found that fishes in a river die) it mayb$os6ible by mean of this method to find out exactly what compoundo are responsible for the death. For this reason, I will go into cone details with this method. In tho actual case we took the extract from 20 mg eagle and concentrated NEV 106554 WATER PCB-00051055 It m such as poeolble and aad@ an injection on the gas ehroB&tograpb oomblnod T/ith the Mae spectrometer. The result was the chronatoGrura thorn on the next slide* Every timo the reeordor showed that a conpound is loaving the column, the effluont is led to the mass epeotromotor. How Juet fen words about the moss epee. Tho Doleoules leaving the column ore bonded with sleetrons at E. Vo have non got tho molocule positive charged, but with tho some aaae as before. This H+ is aeeolereted in a vacuum and will then get a kinotlc enorgi. . where la the apoed. Host eomot the mognetle field that . tries to bend the direction of the molecule. This will bo big for a small moleoule and less for If ws have a alove in the other end we can direotly read the molecular weight. Added to this parent molecule it we will also get addition in formations, baoauaa of the fact that U+ may not be etbbla, a port of them will be broken down before they reach tho sieve in the other end. F.ax. H B bdi . 0C1j Mass apeotrogrome from the different unknown peaks In the eagle sample as shown. The maee numbers equal to ths Molecular weights of the unknovmo could be reed to 426,792, 358, 324. Astonishingly, the molecular diffe rences were constantly 34 maee units. This difference shows a fomilcrity in origin of the unknown. How the fact le that chlorine exeleta ee a mixture of two leotopee with atom weight* 35 and 37 in proportion 75* 25. If , ( the moleoule hat one chlorine, this will give two moleoule peako, one for . Cl/./, and one for C1r._ . If there are two chlorine we have the possibility of one with only 01j^, one with both 01^ and 37 and one with 2 01^ end therefore NEV 106555 WATER_PCB-00051056 e oo The relation of tho poako found on tho different maoo opec woro: Molecular weight 324 358 392 426 Chlorine content 5 . -6 .. 7. _ 8 An explanation of the familiarity of the compounds can be giron if one substance la built from the former by substituting a hydrogen with chlorine IK H* 01, 801 HC1 u\ 34 Then it la possible to calculate tho molecular weight of the parent hydrocarbon fHC. Mpjjp m M - x + X Mjj , where U le the moleoulor weight of the component haring x chlorine atoms. P.ex. for m 426 and 8 Cl we will get tsgse . 426 - 280 + 8 154 and equal with tho other molokyla. The moat probable formula with carbon and hydrogen giving this molecular weight is C^2 H,0 and this can only be aatlcfled when the paront-hydro- earbon is biphenyl, and the unknown being polychlorinated biphenyls. This explanation was later fully verified by injection of a synthetic PBC on the mass epee. furthermore extensive gas ehromatographio investigations proved that the TOC standard gave peaks with the oame retention time as the unknown peaks from the sea eagle. With the method just described I suppose that we have a new possibility to atudy the residues in the air because the pine needles can allweys bo . We have had great difficult; in quantifying the PCB, but when getting a little more time it will be possible. We have done a few calculations on a few species, and I suppose they are right within a factor 2. We have found the residue to be from * It baa been my statement here to-day to present this method for studios of defiling of the nature, and with this method a new typo of defiling agento baa been found to be preaont in nature, and a few experiment have shown where'they may be found. How this method la going to be ueod in the first hadn to aatimato how the situation is in nature as a whole, and in the other hand to find tho leaks throug wbioh they find its way to nature. 8oea maybe are proaont here today to get news about the leaks, and to then I want to ony come back in a year. NEV 106556 WATER PCB-00051057 9. OO So much I think Z can soy again that the FOB hardly can como from agriculture. Ao support for thio euggeotion 1 can any that we hove found FOB in oaglo foathero iron Rlkomueeot fron 19441 where hardly any ehlorinatod postieldes were used in agrloultrue. One sore thing that 1 find icportant to any le that in contrast to the mercury problem this does not aoon to be * pure Swedish problem. I have Just studied ehronatograno takon fro* tendon air, and they clearly contain PCB, and dr. Holdon bao told bo that ho also find then in hie fiohseaploo. But finally in waiting at Boro results Xvshould liko to point0}}?!* aorething. It is provod that ye: oobos to naturo, wo dent hnow now where they are usod, but they ere vory persistant to chemicals and to firs. I think the poison Jury should try to state that a content of FOB shall always be found in an open declara tion. NEV 106557 WATER PCB-00051058 WATER PCB-00051059  Mn o%a# 5? 6 % % VQ>, <% $ tv V r> ? is V) *) <5 V N N X, 3Lo NEV 106559 WATER PCB-00051060 WATER PCB-00051061 s Curve 1 ... * . 5 * .. , $ .S %K ^ Curve 2 > . . - ^ s v> V 5? Q ` S' ' % % % t\ s Curve 3 ,, Curve * * ' NEV 106561 i 7 WATER PCB-00051062 WATER PCB-00051063 o I o li k%f $ x> m ~C-tte/ CL --C-tv rv & j l jok' > o> y> * v NEV 106563 L/A/DRA/e WATER_PCB-00051064 pJ)Cf>P o o/ NEV 106564 4;) WATER PCB-00051065 WATER PCB-00051066 WATER PCB-00051067 N6V 106568 WATER PCB-00051068 .--? ...I. I* f RR J o. NEV 106569 WATER PCB-00051069 a *is & * \ ft 0 %\ c ' fi K i ^ gj * s .HU a- w f ^ /, <js .t / J T~T C) @ V IN 5*?0 \0t' WATER PCB-00051070 r. , V ^ K* .fe & I- Sr O (I yi' "V X1 NEV 106571 WATER PCB-00051071 o L.X > * k* * & o ft 5> $ J ir~z Ot NEV 106572 WATER PCB-00051072 esc/' oo { MEV 106573 WATER PCB-00051073 o e^. -<*?' 5 o < | Vi* e_r "d 3 *w a* 4. .. *. i i^> y. J o ^ C\ 5$ ** 0 **l. ,. *. t I i i iI II NEV 106574 \ WATER PCB-00051074 ,/ Monsanto ......,*-6 i.ecAtipMi p;t f wheeler - St, Louis <$ e*iiL September 11# 1968 rp CCl Dr. R. E. Kelly J>r.._.Scott Tucker proposed Protocols for ^rgbipr/^Tox 1 c 1 ty v Hr. R. ?KeTlerl Studies at Industrial io-Test Lab. ^Mri'^Cummlng Baton -- TO : Dr. W. R. Richard. Attached Is a copy of a letter from Industrial Bio-Test and proposed protocols for Aroclor toxicity studies. This arrives Just as I am leaving for two weeks. I will take this material with me and if possible send you my comments before the end of next week. If it appears desirable to have a session with Dr. Kelly and Bill Hunt to discuss this matter before I return, I am sure Dr. Kelly will be happy to see you. ' EPW:cjs f,`i Wheeler I^ ^72"" .30 < 10 BtV <1... . ^ DEPOSITION : ' j EXHIBIT . I 3dL NEV 167288 WATER PCB-00051075 SndUtdUfal BIO**TE$T ^cUoia/oue^ Sftc. 1610 FRONTAGE ROAD NORTHOROOK* ILLINOIS 60062 AIA CODE lit Tlif^HONE I?t*t010 September 9, 1968 Mr. Elmer P. Wheeler Monsanto Company $00 N. Lindbergh Blvd. " St* Louie, Missouri 68166 ! t ' Dear Mr. Wheeler: I am submitting a collection of protocols for studies with Arodors,. The studies proposed, with prices, are as follows: z: % I. Rat Tissue Study s'`-. *4 Arodor 1 2 levels Aroclor XI 2 levels Aroclor 111 2 levels Toxraphene 2 levels Controls Total $2,700 Additional reference materials could be Included for $600 per material (2 levels). This price is exclusive of analyses. If you choose for us to do all or part of the analytical work, we could work on a cost plus basis or we could pro vide you with'a quotation after we have run through the method. We found no really useful information In our scan of the literature on the metabolism of chlorinated pesticides, I feel that we can get much informa tion from analysis for tissue residues and from study of urine and feces collected from treated animals. It is not possible to quote tor such studies in the absence of fore-knowledge of findings. This could be set up on a cost plus basis with provision to review after the expenditure of a defined sum. One should be able to at least define the problem on a budget of $5,000. ' NEV 162002 WATER PCB-00051076 Mr. Elmer P, Wheeler September 9 1968 Page 2 H. Chicken Toxicity. Reproduction and Meat and Egg Residue Study Three Aroclors with common controls Exclusive of'yaUn`a l'ytical costs HI. Mallard Puck Study- - - - - - $15,000 . Three Aroclora .with common controls^ _ Exclusive of. analytical jsosts $5,000 . IV. 3-.Gene ration Reproduction Study in Rats Three Aroclore with common controls o V. 3-Year Chronic Toxicity Study in Rate Three Aroclore with common controls VI. 3-Year Chronic Toxicity Study in Dogs Throe Aroclore with common controls $35,000 *< ' -1-. $57,500. ' ` ' *4 $85,000 `t ` VII. Subacute Pish Toxicity Study We have not done such a study but we have built one apparatus which allows Investigation of as many as five concentrations of one material plus controls simultaneously for extended periods of time, starting with flngeriings and continuing through a reproduction cycle if this Is desired. * '' If one wanted only to measure the accumulation of test materials over a 90-day period, the cost,' using 5 concentrations, would be ap .. proxlmately $1,500 p6r species for one material, exclusive of analyses. Extending the study through a reproduction cycle would cost an addition . al $3,500. . In any of those studies, material (urine, feces or tissues) could be retained for analysis to determine species differences relative to accumulation and metabolism. . '' NEV 162003 WATER PCB-00051077 o M r. Elmer P. Wheeler o September 9 1968 Page 3 The cumulative cost of the defined studies, exclusive of analytical costs and fish studios , amounts to $200,200. . ' As Dr: Calandra has told you,' billings could be arranged to accommodate to your budgetary needs. <"*----------- .Your comments on this program will be welcome and-should further per-r son^l discussions seem desirable, vre will be glad to moot with you either here or in St, DouisJ .. *_ Sincerely yours, P4^.t.n Otis E, Fancher, Ph. D. Director It - *-Mr OEFiDMS enc* * % . NEV 16200% WATER PCB-00051078 9*idu4bioJ' BIO - TEST Ja^HaU'ued', Snc. t810 FRONTAGE ROAD . .NORTHBROOK, ILLINOIS 60062 . AIM COOK III ' mtfMONl 1TI-I010 . PROTOCOLS FOR . MONSANTO COMPANY " ` AROCLOR STUDIES ' NEW 1%3472 WATER PCB-00051079 Jhtdtrthial B l O - T E S T ItoMii&ucJ; Sttc. ' t PROTOCOL. FOR , MONSANTO COMPANY . , A TISSUE'RESIDUE STUDY IN ALBINO RATS 1. . WITH AROCLORS 1. Outline of Experiment . A. Type and Length: Tissue Residue Study; duration 30 days Animal Species Tested; Male Albino Rats (approximately 100 g) C. Organization of Groups; '' Group Number of Animals Male Female Dietary Concentration in ppm Control ` 1 n 15 . ' ; '15- . None 15 15 . . . Low.dose level ' 15 . 15 ' High dose level D. Test Material Administration . ' ' Diets will be prepared fresh weekly by mixing the calculated quantity of test material with a standard pulverized rat ration. Food will be allowed ad libitum. _ ': II. Parameters to be Studied ` ' - : ?* '. . , A. Feed Consumption ' ' ' Feed consumption will be determined weekly for each animal. Reactions . ' ' . Observations for untoward behavioral reactions will be made. '. NEV 143473 t WATER PCB-00051080 r$iuli<iiAial B 1 O - T E S T " ImaioAM, Hhc. 2 C. . Gross Pathology ' . Upon sacrifice, organs and tissues will be examined grossly for pathologic alterations. _ # *o ' _' . 111. Sample Collection At the end of 30 days all animals will be sacrificed and samples of muscle, fat, liver and kidney will be; taken from each animal. Samples e of each tissue from each animal will be frozen and will either be shipped to Monsanto for analysis or analyses will be done by Bio-Test. OEFiDMS 9-9-68 NEV 14347% WATER PCB-00051081 SudmUial B I O - 1 I; S Y " -Zio^aioAicS, Pnc, PROTOCOL, FOR ' . MONSANTO COMPANY CHICKEN TOXICITY, REPRODUCTION AND RESIDUE STUDY ON AROGLOR . s'. The object of the study will be to investigate the general toxic effects of the test material on young adult male and female chickens with special emphasis upon hatchability of eggs and viability of offspring. In addition, ' samples of meat and eggs will be analysed for test material residues (either by Monsanto or by Bio-Test). . Sixteen male and 80 female 12-week old white Leghorn chickens will be selected'for the study. These animals will be equally-divided into one control and three test groups. The three test groups will correspond to graded dietary levels of the test material. Dosing will begin immediately and will continue through the egg collection period. . . The chickens in the control and test groups will be weighed weekly and observations for mortality, reactions and general food disappearance . will be made periodically during the study. ' _ As each group begins laying (at 17 to .18 weeks of age), the eggs will . be collected daily and egg weights recorded. When the egg weights are consistently between 50 and 60 grams, and at least 20 per cent of the hens are laying, the daily egg production will be collected and placed in an ' incubator tray. Egg collection will be continued for 28 days from collection NEV 143475 " ' .' WATER PCB-00051082 B I o - T E S Y tMaiMiai, Sue, 2 Day One or until at least 100 eggs per group are available for hatching. 0 During the storage period (not to exceed live days lor any group ol eggs), the eggs will be turned twice daily. The eggs will be placed in an incubator maintained at 99 to 100F with a wet bulb reading of 85F. The egg production lor an additional week will be collected lor analysis. Total egg production and egg weights will be recorded. At the end of the egg collection period, one-half of the chickens in each group will be sacrificed, defeathered and quick-frozen. The car casses and the eggs retained for analysis will be shipped to Monsanto or will be retained for analysis at Bio-Test. . The remaining chickens will be placed on a 30-day recovery regimen during which time the test material will be removed from the test diets. Eggs will be collected once each week. At the end of this period, the re maining chickens will be sacrificed and handled in the same manner as those at the end of the test feeding period. The carcasses and eggs will again be ` retained for analysis. ' .1 The chicks from the first generation will be observed for 30 days post-hatching. . . ` * ; RJPsDMS O 9-9-68 NEV 1*3*76 WATER PCB-00051083 Sndu^Aial B 1 0 - T E S I ktaknlGi., $nc. PROTOCOL FOR MONSANTO COMPANY .DUCK TOXICITY AND.RESIDUE STUDY ' ON AROCLOR The object of the study will be to investigate the general toxic effects of the test material on young adult male and female mallard ducks and to' determine residue levels in specific organs and whole carcass. Twenty male and twenty female young adult mallard ducks will be selected for the study. These animals will be equally divided into one control and three test groups. The three test group's will correspond to graded dietary levels of the test material. ' * ' The ducks in the control and test groups will be weighed weekly and observations for mortality, reactions and general food disappearance will be made periodically during the study. At the end of a 30-day feeding period, one-half of the animals in each group will be sacrificed, defeathered and subjected to a gross pathological . examination. The liver, kidneys and samples of skeletal muscle and fat will be removed from each bird and packaged separately, These tissues will be quick-frozen and retained for analysis for the test material The remaining ducks will be placed on a 30-day recovery regimen during which time the test material will be removed from! the test diets NEV 143477 WATER PCB-00051084 SndiuUial B i O - i E S T Site. 2 At the end of ths6 period, the remaining ducks will be sacrificed and . handled in the same manner as those at the end of the test feeding period. i ; .. . # RJP:DMS. 9-9-68 NEV 143478 WATER PCB-00051085  Jiiduikial B 1 O - 1 ESI J<~ 'vtatoAioi, fac. O PROTOCOL FOR MONSANTO COMPANY THREE -GENERATION REPRODUCTION STUDY ' OF AROCLOR ' IN ALBINO RATS . I. General ' _ A three-generation reproduction study will be conducted with Sprague-Dawley derived albino rats. A total of 96 weanlings (32 males and 64 females) will be equally subdivided into three test groups and one control group. The three test groups will correspond to the feeding of three graded dietary levels of the test material, . ; II. o II. First Generation . A. Parental Animals 1. Diets and Feeding ' '' . `. All diets will be prepared in the'central diet room of the laboratories. The basic ration with which all diets are prepared is a standard, pulverized rat stock diet*. The diets for any given test group will be prepared by adding a calculated weight of the test material to a pre-weighed portion of the stock diet. ' . The amount of food allotted per week to each rat is to be sufficient for ad libitum feeding. However, checks will be made daily to ensure that the food jars are not empty. . NEV 143479 9 * Purina Ral Chow, Ra.lslon Purina Company, f*i,, jUmt.*, MJnsonvi, WATER PCB-00051086 hiduikial B I 0 T S I laUtatMUl. Shc. 2 2. Dody Weights and Weight Gains . . The body weight of each rat in every group will be deter- ,4 * ' ' i . ' mined and recorded initially, and weekly thereafter until the animals . ;' are 100 days old, ' '' ' 3, Mortality, Reactions and General Observations ' Mortality and abnormal behavioral reactions will be recorded daily. The animals also will be observed for fertility, length i '. - * * . . ,. of gestation and lactation performance, '. 4, Mating Procedure When the animals reach 100 days of age, each male will ' be randomly mated with two females from the same group. After suc cessful copulation, determined by the presence of a copulation plug or blood in the vagina, the male will be removed from the females and returned to his original cage. Any male failing to copulate within two cstrus cycles of the female will be replaced by another male of the same group. However, no more than two males will be used per female during a given breeding cycle. Records will be kept of the number of successful 6 . : ' copulations observed, the number of estrus cycles required to obtain a ; ' mating, and the number of resulting pregnancies. These data will be !j:- utiliz-cd to calculate mating and fertility indices. . The Fla litters obtained will be weaned at 21 days post- t . partum. The females will then be given a 10-day rest period and again ! ' ' mated, the above procedure being repeated to obtain Fib weanlings. i. ' ' .. ^ '' NEV 1*3480 WATER PCB-00051087 UndnlOual B 1 0 T E 5 T lalmafatiei; Sue. 3 5. Pathologic Studies . . After the second litter has been weaned (following approx imately 33 weeks on test), 8 male and 8 female animals from each group will be sacrificed and gross pathologic observations will be made. Organ weights will be taken on the liver, kidneys, spleen, gonads, heart, brain and any organs which appear abnormal. A complete set of tissues will .f be removed and fixed in a ten per cent formalin solution. In addition, microscopic examinations will be conducted upon five males and five females from both the control and the high test groups. If abnormalities are noted, the affected organs of the lower test group animals will also be examined. . % NEV 1A3*81 WATER PCB-00051088 {/tuluiUial B I 0 T E S T laltwitMUi, Sue. 4 O o o The following tis sue s and organs will fee examined: Tissues and Organs Examined Grossly Tissues and Organs Examined Microscopically . Heart Trachea ' Lungs . Liver Pancreas Esophagus Stomach Intestinal tract * Spleen Lymph nodes . Kidneys Urinary bladder Testes Ovaries Prostate Seminal vesicles Uterus Pituitary gland . Adrenal glands Salivary glands Thyroid glands Skeletal muscle Bone Peripheral nerve Eyes Brain _ Thymus . Optic nerves Aorta ' Spinal cord Heart (right and left ventricles) Trachea Lungs . Liver '` Pancreas Esophagus ` Stomach (cardiac, fundic and pyloric regions) `' Small intestine (duodenum, / *' . jejunum and ileum) . Caecum . Colon ' Spleen Lymph node (cervical and mesenteric) Kidney ^ ._ ' , Urinary bladder ` Testis :. Ovary ' ." . Prostate Seminal vesicles '. Uterus . Pituitary gland Adrenal gland Salivary gland (submaxillary) Thyroid gland Parathyroid gland Bone marrow (sternum and femur) Peripheral nerve (sciatic) Brain (cerebrum, cerebellum and pons) . Spinal cord (three levels) ' Post-mortem animals will be examined in the same manner but organ weights will not be recorded, . *. Throughout gross and microscopic examination, particular attention will be paid to the reproductive organs, .. . ' NEV 143482 WATER PCB-00051089 3tuLuiual BIO-TEST JoUmUu'&t, hx. ' ' . ' 5 B. Progeny . .' ' . . . 1. Body Weight Data ' ./ . ' Pups will be weighed at weaning. ... a. , 2. Mortality, Reactions and General Observations `` All pups will be examined for physical abnormalities at ; birth and the number of viable and stillborn members of each litter recorded. Records of survival at periodic intervals during the lacta. #* . tion period will be maintained and a final examination for physical abnormalities will be made at the weaning of each litter. ' ' 3. Survival Data . Survival indices will b.e calculated for various points during the lactation period. On the fifth day of lactation, litters of greater than 10 pups will be reduced to that number. 4. Pathologic Studies . A gross internal pathologic examination will be made upon any pup appearing abnormal. No such examinations wiil be made upon progeny which appear normal. ,. . ' ' % 4. ' * III. Second and Third Generations _ . The procedures followed for the second and third generations will . be identical to those described for the first generation except that the _ parental animals for the F2 generation in each group will be selected from Fib weanlings of that group. Parents for the F3 generation will be selected from F2b litters. . ' . . . . ; ' ' NEV 143*83 > WATER PCB-00051090 Siiduil'Ual B 1 O - T E S T lalmatcydai, htc. 6 In addition, ten male and ten female pups from the F3b litters of each test group and the control group will be sacrificed at weaning (21 days post-partum) and subjected to complete gross and microscopic . . 4 * examination. ' ' IV. Reports . A complete formal report will be submitted upon completion of each generation. # * ' MLK:PSH 9-5-68 NEV i*3*84 WATER PCB-00051091 SiidirtUioi B I O - T E S T / 'oictiviiei, Site. PROTOCOL FOR MONSANTO COMPANY I TWO-YEAR CHRONIC ORAL TOXICITY OF ' AROGLOR ; IN ALBINO RATS 1,, Outline of Investigation '. A. Type and Length: Two-Year Chronic Oral Toxicity B, Animal Species Tested: Charles River Strain Albino Rats G,, Organisation: .. Group Control Test I Test II Test III Number of Animals Male Female * Dietary Level of ' Test Material .. . (ppm) 30 . 30 . . ..None Administered 30 30 . Low Level ' 30 30 ' Middle Level 30 30 High Level D. Means of Administration: Voluntary oral Ingestion; ad libitum feeding of diets containing various levels of test material, JL Parameters To Be Investigated A. Body Weights NEV 143485 A)J animals will be weighed weekly during the first three months oi the study and monthly for the remainder of the two-year test period. . WATER PCB-00051092 SttdtiiiAial B I 0 - Y E $ T lal&ialotiti. Sue. 2 B. Food Consumption ' ' .' Weekly food consumption will be recorded for the first three months of the investigation. Thereafter, monthly spot checks will be . made. .. ' ' ' C. Mortality and Reactions ' Checks for mortality and untoward behavioral reactions will be conducted daily. . D. Hematologic Studies, Clinical Blood Chemistry Studies and ' Urine Analyses . The studies listed below will be conducted on five rats of each 6ex from the Control Group and Test Group III at the beginning of the study and after 3, 6, 9, 12, 18 and 24 months of feeding: ' 1. Hematology: Hematocrit value, hemoglobin concentration, erythrocyte count and total and differential leukocyte counts. 2. Clinical Blood Chemistry: Blood urea nitrogen concentration ,. (BUN), serum alkaline phosphatase activity (SAP), blood glucose concentration and serum glutamic - pyruvic trans ' aminase activity (SGPT). ' 3. Urine Analyses: Albumin concentration, glucose concentra- _ . tion, microscopic elements examination, pH determination and specific gravity, _. . The above listed studies will be conducted on animals in the . lower dose groups if significant findings appear among high dose animals. * , * " NEV 1*3*86 WATER PCB-00051093 Stxbdkid B I 0 T E 5 T lakteiortei, Stic. 3 o I 5 o E. Pathologic Studies ' 1. Gross '. Complete gross autopsies will be conducted upon all post mortem animals unless precluded by post-mortem autolysis, all animals sacrificed in extremis, five males and five females from each group sacrificed after three months of testing and upon all animals surviving 24 months of testing. At the time of each autopsy, representative tissues * and organs will be taken.and fixed in 10 per cent formalin solution. Absolute organ weights will be recorded and organ - body ' weight ratios and organ - brain weight ratios will be calculated and sub jected to statistical analysis, viz. Analysis of Variance and/or MtM-tests, The following organs will be included: liver, kidneys, s pie on, gonads, heart, brain and any other organ appearing abnormal upon gross examina tion. 2. Microscopic Microscopic examinations will be conducted upon tissues and organs taken from selected animals sacrificed in extremis, and five males and five females from the control and highest dietary dose groups sacrificed after three months and 24 months of testing. The tissues and organs to be examined will include: heart, liver, lung, pancreas, stom ach (cardia, fundus and pylorus), small intestine (duodenum, jejunum and ileum), caecum, colon, .spleen, lymph node, kidney, urinary bladder, testes, ovary, prostate, uterus, pituitary gland, adrenal gland, salivary '* ' . . . . . '' . .1 v NEV 1434B7 . ^' r WATER PCB-00051094 StulnUud B I 0 - T E 5 T lat&naittiU, Snc, 4 gland (submaxillary), thyroid gland, parathyroid gland, skeletal muscle, bone marrow, peripheral nerve, trachea, spinal cord, eye, optic nerve and brain (cerebrum, cerebellum and pons). Any significant tissue or organ changes at the high dose level would also be examined at the lower levels. F. Reports . . . Interim status reports will be submitted after 3, 12 and 18 .* . .months of testing. These reports will contain pertinent data collected to that date. . . . At the conclusion of the study, three copies of a final formal . report will be submitted, ' ' . Ml.KrPSH 9- 5-68 : NEV 143488 WATER PCB-00051095 ..frdidiAial B i O - T E S T Jalu*iat>*ic4, Sac. :s Ii* o PROTOCOL FOR MO N SAN% TO COMPANY TWO-YEAR CHRONIC ORAL TOXICITY '. .OF ' AROCLOR ' IN BEAOLE DOGS : I.. Outline of Experiment '' ,' _ . A. Type and Length: Two-Year Chronic Oral Toxicity . ' B. Animal Species Tested: Pure-Bred Beagle Dogs 0` C. Test Material: Aroclor *. ' . . . D. Organization: Three Test Groups and One Control Group 1. Number of Dogs/Group: Eight (four males and four females) 2. Dose Levels: Control Group - None . Test Group I - Low level .. Test Group II - Middle level Test Group HI > High level 3,, Means of Administration: Voluntary oral Ingestion; ad libitum .. ; ' feeding of test material In diet. i R, Parameters To Be Investigated ..... ' . . . . A. Body Weights ' * ' - . / '. . All animals will be weighed weekly. . ' .; B. Food Consumption Weekly food consumption will be recorded. C. Mortality and Reactions Mortality and untoward behavioral reactions will be recorded daily. ' NEV 143489 WATER PCB-00051096 4 * fridulitial B I O - T E S T . Maiydai-, Sac. D. Hematologic Studies, Blood Chemistry Studies and Urine Analyses The studies listed below will be conducted upon all dogs prior to the inception of the test, after lr 3, 6, 12 and 18 months of testing and i * ' . just prior to its conclusion. . 1. Hematology: Hematocrit, hemoglobin, erythrocyte count,' . and both total and differential leukocyte counts. * 2. Blood Chemistry; Blood urea nitrogen, blood glucose, serum alkaline phosphatase, serum glutamic-pyruvic transaminase . and serum glutamic -oxalacetic transaminase. . 3. Urine Analyses: Albumin, glutose, pH, microscopic elements ' and specific gravity. ' . 'I ... O E, Pathologic Studies . 1. Gross Pathologic Studies . ,' Complete gross autopsies will be conducted upon animals sacrificed in extremis and upon all post-mortem animals during the inves tigation. At the conclusion of the 24-month study, mil surviving dogs will be sacrificed and examined. At the time of each sacrifice, a complete set of tissues will be removed from each dog and preserved in ten per cent formalin solution for histopathologic examination. Also at the time of each sacrifice, the weight of the jliver, kidneys, spleen, gonads, thyroid, adrenals, pituitary and heart will be recorded. ' 2. Histopathologic Studies _ NEV 143490 I. Histopathologic examinations will be conducted on tissues . . i. . ' ' taken from animals sacrificedj.nlaxtr emls, from post-mortem animals WATER PCB-00051097 $,iditiirUat D l O - T E S T - tyiatyOci; Sttc. 3 and from all animals sacrificed after 24 months of feeding. The tissues to be included in the examinations are as follows j lung, heart, liver, pancreas, mesenteric lymph node, stomach (cardia, fundus and pylorus), ' ' small intestine (duodenum, jejunum and ileum), colon, caecum, kidney, adrenal gland, urinary bladder, testes, ovaries, prostate, thyroid gland, submaxillary salivary gland, parathyroid gland, uterus, brain (cerebrum, cerebellum and pons), bone and bone marrow (femur), and skeletal muscle (gastrocnemius). * * . ` . . F. Reports . * Interim status reports will be submitted after 3, 12 and 18 months of testing. These reports will contain pertinent data collected to that date. . At the conclusion of the study, three copies of a final formal report will be submitted. .. '. MLKsPSH 9-5-68 i NEV 143491 WATER PCB-00051098 December 20, I960 Dr. Jooepb C* Calandra Industrial Dio-Test Laboratories, Xtyc. 1810 Frontage Road ' Northbrook, Illinois 60062 Pear joe i rfp. This letter authorizes the Initiation of two of the proposed Arcelor studies as followst Project No. BTL Aroolor X-Fowl - Gross Toxicity la * Aroolor 1242 lb - Aroolor 1254 Io - Aroolor 1260 Id - Aroolor 5460 ie - Toxaphene If - DOT Xg - Chlorinated naphthalene The protocol for these studies is to be eonsietent with our discussions when you were in St Louis and X would appreciate receiving a note from you outlining what you plan to do with an approximate oost. Project Wo BTfc - Aroolor XX - 30 Day Rat Tissue Study XX& - Aroolor 1242 XXb - Aroolor 1254 XXo Aroolor 1260 lid - Aroolor 5460 lie - Toxaphene Ilf - DOT . XXg - Chlorinetd naphthalene . DEPOSITION EXHIBIT 35* 2-/r-n NV 008162 WATER_PCB-00051099 Dr. Joseph C. Calandra -2- December 20, I960 These studies sro to be carried out as proposed In your protocol submitted with the letter of Dr. Fancher dated September 9, 1968. That letter Indicates a coat of $2,700 for three of the Aroclors, Toxaphsne and controls. Further It indicates that additional materials could be Included for $600 per material. Since we are adding additional Aroclor, DDT and chlorinated naphthalene X assume that the rat tissue study will cost approximately $*4,500, We arc obtaining samples of several chlorinated naphthalenes and will provide you the material to be investigated. Do you have a readily available source of DDT or shall I get this for you through our Agricultural Chemical Oroupt I have enclosed s copy of my summary of our meeting when you were down here (as you and X discussed it). There Is also a copy of Dill Richard's version* 1 hope you have licked the flu bug and will hsve a happy holiday. ftlnoerely. Elmer ft. Wheeler Manager, Environmental Health EfWtcJs Enclosure cci W. ft. Richard ft. E. Keller/flcott Tucker,; C. Faton w. Ku Johnson ft* E. KellyA* H. Hunt NEV 008163 WATER PCB-00051100 April 8, 1970 Herbert BlUMnthal Ph.D. Chief, Petitions Review Branch Bureau of Foods# Pesticides and Product Safety U. S Food and Drug Administration 200 C Street, Southwest Washington, D* C. 20204 Dear Hertn Confirming our telephone conversation 1 have enclosed Xerox copies of the status report* for tha chronic toxicity studies for our Aroolors at Industrial Bio Test, Inc* Specifically, three of our polychlorinated biphenyl* are under Investigation* Thess are Aroolors 1242 biphenyl chlorinated to the extent of 42^1# 1254 (biphenyl chlorinated to the extent of 5V' # and 1260 biphenyl chlorinated to the extent of 60% Studies Include two year oral administration to rats, two year oral feeding to dogs and a three generation rat reproduction study* As indicated in the enclosures, the levels of admin istration are 1, 10 and 100 ppm for each of the com pounds* Further# the status reports for the chronic dog studies represent data at tha ehd of nine months* The enclosed copies on the rat studies show data if the end of six months administration* As m mentioned on the telephone# we added 30Q rats to the ohronlo studies after the original two year projsot had gotten underway to allow a sufficient number of animals for sacrifices at three# six and twelve months* Hlatopfcthology has bean completed on Urn sacrificed animal* and Dr. Calandra has reported verbally that thers ars no positive pathological findings* 000629 WATER PCB-00051101 Dr* Herbert Blumentha1 April 8, 1970 rag# Two Tho rat reproduction studies are Into th# eeooad gener ation. At this point Or. Calandra hat Indicated that there definitely haa been no effect with any of th# compound* at tha 10 ppa dietary level. Thar# ia tone equivocal poaaibl# #ffaot in tha animals at th# 100 ppm laval with Arcelor 125^. If you have any apaciflc question* after reviewing th# enclosed statue summaries, plesss feel free to call Br. Calandra or Dr. Fanchar directly. Best personal regards. Sincerely, R. Etamet Kelly, K. D. Medical Director REXiJu c.c. Dr. Joseph C. Calandre Dr. Otle 2. Fincher b,c, W. B. Papageorge 0. W. Ingle Knolosurta NEV 000630 WATER PCB-00051102 Monsanto 00 H ' M!ltfltl am: omi M-tooo THREE-OEHERATION REPRODUCTION SWOT IN AIBZNO RATS WITH: AROCLOR 1242 AROCLOR 1254 AROCLOR 1260 RESULTS OP TOE FIRST OQIEMTION September 4, 1970 Submitted by: R. Emmet Kelly, M. D. Medical Director NPC00009503 *4 ' WATER PCB-00051103 [a f f UH**<* I _ } ' | ; ' SruBu&trj&l BIO -TEST JtGhmhwA. Snc. 1010 montage road NORTHBROOK, ILLINOIS *0063 .** . ' '. . . REPORTTO . MONSANTO COMPANY THREE-GENERATION REPRODUCTION STUDY IN ALBINO RATS - AROCLOR 1242 RESULTS OF THE FIRST GENERATION SEPTEMBER 4, 1970 IBT NO. P8797 . 3 / ~J>C009504 WATER PCB-00051104 z i SmUaiVuci BIO -TEST XaimahukA, 3m. 1010 9RONTACE ROAD NORTHOROOK. ILLINOIS 00062 September 4, 1970 l ! Mr. Elmer Wheeler Monsanto Company Medical Department 100 N. Lindbergh Boulevard St. Louis, Missouri 63166 Dear Mr. Wheelers Re: IBT No. P7297 - Three-Generation Reproduction . Study in Albino Rats - Aroclor 1242 We are submitting herewith our laboratory report dated September 4, 1970, prepared in connection with the above study. This report presents the results of the first generation. Very truly yours. -- JCC/kJl ' J. C. Calandra President 9* ' NPC00009505 WATER PCB-00051105 tju'Jjl DiO'T ES T $mc. REPORT TO MONSANTO COMPANY THREE-GENERATION REPRODUCTION STUDY . IN ALBINO RATS - AROCLOR 1242 ' RESULTS OF THE FIRST GENERATION SEPTEMBER 4. 1970 1. Outline of Study IBT NO. P7297 ' ' A. Type and Length; Three-generation reproduction study B. Animal Specie* Taated: Cher lee River albino rate C. Material Toted: Aroclor 1242, Lot No. AK-255 . D. Starting Date: May 8, 1969 E. Statu* of this Report; Completion of the first generation (Fo parents - Fla and Fib progeny) F. Organisation- A structural outline of the experiment la given in Table 1. NPC00009506 WATER J i 8 O T B S I JaUta&tdni. Jtie. 2 Groun C T-I T-11 T-III TABLE 1 ' TEST MATERIALS Aroclor 1242 Outline of Experiment Fo Generation Dietary Level (ppm) None Number of Animals Male Female 8 16 1 8 16 10 8 16 100 8 16 G. Mean* of AdmtnUtration: Voluntary oral Ingeatlon. NPC00009S07 WATER yj 6I0-IEST Itdmaktiei, Sue. 3 jL Summary The first generation of a thrcc-gcneration reproduction study of Aroclor 1242, Lot No. AK-255, at dietary levels of 1, 10 and 100 parts per million has been completed. The following data were obtained during the first gene ration: . A. Progeny fPla and Fib) The numbers of pups delivered and weaned by treated females were generally as large or larger than those from the control group. The survival indices of progeny from treated females were higher than the indices for controls. The lactation indices of the T-UI group, but not tho T-l or T-U groups, were slightly lower than these indices for the control group. All progeny body weights were normal and there were no unusual reactions noted among any offspring- B. Parental Animals (Po) The body weights of the treated males and females were nor mal and compared favorably whb those of the controls. Ona T-111 male died during the pre-mating period;-one T-l female died while lactating for her second litter; one control female died during parturition of her first litter. NPC00009508 WATER \ S BIO*TEST %* 4 Ibo d.u obtained ir.or P*"1*1**1* . tbe.e animala revealed no .ipr, botwa.n ...t and .. control rats. Organ weight dai* studies confirmed the absence e *. -.hr results of the hlstopathologie .. oaihologlc changes which could ? be related to the ingestion of p Matin, indie... l.r.ili: -W. .[ pro,nancy and parturition for treated anir* - `v* re normal and compared favorably to those of control an1-*-** Respectiu *. submitted, ,, Report prepared bv: INDUST R- * B10-TEST LABORATORJES, INC. ^^ I \/\ ^ . vl, \/a--/w f \****' -- 1 JsmeiTv rnup !.* * *'7 . Rat Toxi. * Department 1~ * . leport approved by: M. L. K>- ''rcr* P'iX*3, Manager. ..-Ecology Qj; . * S. Otis E- . i ,`cr* oPhk< Dn.* _ . . , tt.vAP(Af LM 1 September 4. If70 r>.Ajl:psh NPC00009509. WATER PCB-00051109 lO-TlST Il**t**i, 32 4. Rcactlona '^ No untoward behavioral reaction* rt ohitrved among *r test or control progeny. NPC00009S10 0 WATER I ` ,, m* SnduiUial BIO -TEST XaJmah^BA. Snc. 1010 montaoc road NORTHBROOK, IlllNOIS MOM **CA C* ill mcmtm REPORT TO MONSANTO COMPANY THREE-GENERATION REPRODUCTION STUDY IN ALBINO RATS - AROCLOR 1214 RESULTS OF THE FIRST GENERATION SEPTEMBER 4, 1970 ' 1BT NO. P7297 / ' UPC000095H WATER PCB-00051 111 i SnduAOual DIO -TEST Jk&ot&tdtieA. Ate. MIO PRONTAOC ROAD NORTHBROOK. ULINOIS 6006J September 4, IfTO Jr. Elmer Wheeler '.,n*anto Company *'fical Department ; N. Lindbergh Boulevard % Louie, Missouri 43166 Iv*r Mr. Wheeler: . . Re: 1ST No. P7297 - Three-Generation Reproduction Study in Albino Rats - Aroctor 1214 We are submitting herewith our laboratory report dated `.ember 4, 1970, prepared in connection with the above study. This report presents the results of the first generation. . Very truly yours, ` Pt. . ' :c/kji J. C. Calandra President | ., 'l UPC00009512 WATER PCB-00051112 510 T E S T ImowlMA'J, Jttc. REPORT TO ' MONSANTO COMPANY THREE-GENERATION REPRODUCTION STUDY IN ALBINO RATS - AROCLOR .1114 . RESULTS OF THE FIRST GENERATION Outline of Study SEPTEMBER 4, If 70 1BT NO. P7297 A. Type and Length: Three-gen*ration reproduction study B. Animal Specie* Tested: Charlec River albino rata C. Material Teated: Aroclor 1214, Lot No. AK-38 D. Starting Date; May 8, 1969 E. Statua of thla Report: Completion of the first generation (Fo parents - Fla and Fib progeny) F. Organisation; A etructural outline of the experiment ia given . In Table 1. NPC00009513 i WATER PCB-00051113 DIQ -T E S T JaUwlttiei, %& 2 roup 1 41 411 TABLE I TEST MATERIAL? Aroclcr 1254 Outline of Experiment Fo Generation Dietary Lavsl (ppm) Number of Animals Male Female 9 None 1 8 16 8 16 10 ' 8 16 ' 100 8 16 G. Meant of Administration: Voluntary oral ingestion. NPC00009514 '$ WATER ..J, BIO-TEST leUaiHitk fa 1 e It Summary .. ' . The Cf*t gene ration of * lhrcege: oration ^'production study of Aroclor 1254. Lot No.AK-38. t dietary levels of 1, 10 and 100 ppm M, been completed. The following data were obtained during the first generation: ' A. Progeny ' The data, from progeny of females fed cither 1 or 10 ppm were normal In all respects. ' Although no adverse findings were noted lu lira first litter of females fed 100 ppm. the number of pups delivered tnd weaned for the second Utter was slgnificently lower then normal. The survival of pup, that were delivered was slso significantly luw,r than normal. In view of these findings, the females fed 100 ppm remitted for a tSird Utter. The data from this litter substantintd the findings noted : the second litter. / ,` ' B. Parental Animals ', Females fed 100 ppm gained slightly less weight that did eetrols. Males fed 100 ppm and all rats fed UW I t,r 10 ppm *tUbUed weight gains which were not different Ituu, Tere were no deaths which could be related to lira gains. J Aroclor if, and no unusual behavioral reactions were , Cross pathologic examinations revealed w. " vs between test and control rats. differ* NPC00009515 WATER_PCB j ,, f i S T .*>4/sX, A*. 4 .SMiiolUal .-natv vr upon organ weight data revealed several .mi difference a. Significantly higher liver to body weight ratir.s ,-r.**rded for all rats aed 160 ppm, however the absolute weights . .^nificantly higher o.ily in males. Males fed 1 or 10 ppm exhlfe- significantly lower liver weights and liver to body weight ratios. .rvation of thyroid weights was noted for both males and females : :o ppm. Histopathologic examination of tissues and organs revealed .di'.is in three of five males. No other significant differences noted between test and control animals. The mating index for the third litters of rats fed 100 ppm was . Sow and, in the second matings of these animals, three females rbed their litters. All other mating indices, fertility indices, r.ces of pregnancy and parturition and mean gestation times were r:n.il. Respectfully submitted, INDUSTRIAL BIO-TEST LABORATORIES, INC. prepared by: jf\ Ja^nis li. Plank Croup Leader Rat Toxicity Department NPC00009516 WATER PCB-00051116 OlO-T GST Stic. SZ 4. Reactions No untoward behavioral reactions were ebserved amon{ ithcr lest or control progeny* NPC00009517 .i. WATER '.. 9tvSu&0ual DIO TEST 1B0 FRONT ACC ROAD. NORTHBROOK. ILLINOIS A00A2 Sac. . REPORT TO MONSANTO COMPANY THREE -GENERATION REPRODUCTION STUDY IN ALBINO RATS - AROCLOR 1260 RESULTS OF THE FIRST GENERATION SEPTEMBER 4, 1970 . IBT NO. P7297 ' .' ! i i j ii ! I j ' *i 8 I I NPC00009S18 i 1! I : I WATER_PCB-00051118 SnduAUici BIO -TEST J!<U*itoJtyucA. 3m. 1B10 SSONTAGC ROAD NORTHBROOK. IUINOIS 00062 ' September A, 1970 I I ' Inter Wheeler nte Company 1 Department Lindbergh Boulevard ais, Missouri 63166 tr. Wheeler: . Re: IBT No. P7297 - Three* Gene ration Reproduction Study in Albino Rata - Arcelor 1160 We are submitting herewith our laboratory report dated ber 4, 1970, prepared in connection with the above study. This report proaents the results of the first generation. Very truly yours, P Xt> ---- -r - . J. C. Calandra President ' NPC00009519 I II iIiI i i I I I t I WATER_PCB-00051119 SOFTEST Jal+\afaU(4, jut. i i i REPORT TO MONSANTO COMPANY THREEGENERATION REPRODUCTION STUDY IN ALBINO RATS - AROCLOR 1260 RESULTS OF THE FIRST GENERATION SEPTEMBER 4, 1970 IBT NO. P7297 Pullin'* of Stu<?y A. Tyoc and l.cnrth: Three-gene ration reproduction study D. Animal Species Tested: Charles River albino rats Materia! Tested: Aroclor 1260, Lot No. AK-3 3. Starting Date: May 8, 1969 '- 2. Stilus of This Report: Completion of the first gene ration (Fo parents - Fla and Fib progeny) * OrcnnlsAtinn: A structurnl outline of the experiment is given in Table I. 4i i I i ii i i I iI NPC00009520 i!i WATER PCB-00051120 3 - T E S T Jaiowtnioi, Sue* 2 TABLE I . TEST MATERIAL: Aroclor 1260 Outline of Experiment To Generation Dietary Level > {ppm) None 1 10 100 Number of Animals Male Female 8 16 8 16 8 16 8 16 M< .m* of Administration: Voluntary oral ingestion. ! j * j NPC00009521 I \. WATER_PCB- OT ES T St6. 8 Summary The results of the first generation of a three-generation reproduc- study conducted on albino rats fed Aroclor 1260, Lot No. AK-S, at ry levels of 1, 10 and 100 parts per million are presented below. Progeny (Fla and Fib) . The number of pups delivered and weaned by treated femalesa -esentialiy the same es controls. In the second (Fib) litters, s fed 100 ppm delivered slightly more stillborn pups then did ole. Survival indices of progeny from treated females were not ent from the control indices. The body weights of the weanlings treated females were normal, and there were no unusual reactions among any offspring. . Parental Animals (Po) The body weights of the males and females receiving Aroclor m their diet were about the seme as those of the controls. One 1 female died white giving birth during her first pregnancy, were no untoward behavioral reactions noted. ' Cross autopsy conducted upon males and females in ell groups *d no observable changes between test end control rets. The weights and ratios of males fed 1 or 10 ppm were lower than con- while the liver weight* and ratios of males fed 100 ppm were r than controls. Histopathologic examinations revealed no NPC00009522 p I O T E S T /(/iitc/tiwj, }ttc. 4 .angcs in the tiiiuei and organs which could be attributed to the Inges,n of Aroclnr 1260. The mating indices for both litters of rats fed 100 ppm we re wr than control. However, the index for the second (Fib) litter is thin the normal range of the rat strain used. All other mating indlcea, rtility indices, incidences of pregnancy and parturition and gestation ncs for treated animals compared favorably to the controls. Respectfully submitted. INDUSTRIAL BIO-TEST LABORATORIES, INC. port prepared by: Ja{ti^s B. Plank Croup Leader Rat Toxicity Department port approved by: M. L. Keplin^cr. V&D. Manager, Toxicology Otis E. Fanchcr, Ph. D. Scientific Director I \ 9 i I ii i i i i I I ictnlic r 4, 1970 i;pih NPC00009523 a WATER PCB-00051123  TEST JulfixafMifli, %t& 3. P.ciietlom No untoword behavioral reactions were noted among the ai animal a In any group. f Autopsy Findings a. Grogs Autopay Finding* " At the time of sacrifice, gross autopsy revealed no cnees between test and control animals. b. Organ Weights and Ratios Msan organ weights, organ to body weight ratios and . to brain weight ratios are assembled in Tables VI through XUI. NPC00009524 I "f.. WATER tu-sl 010 - T E S T Site. 32 4. Reactions No untoward behavioral reaction* were observed among either test or cost.* progeny. ***000009525 WATER PCB-00051125 4 StuQjuMriUil BIO -TEST XabwcLtcyuzb, Sac. 1810 FRONTAGE ROAD NORTHBROOK. ILLINOIS 60062 November 12, 1971 Mr, Elmer P. Wheeler Monsanto Company 800 North Lindbergh Boulevard St. Louis, Missouri 63166 Dear Mr. Wheelers Re? IBT No. B7298 - Two-Year Chronic Oral Toxicity Study with Aroclor 1260 in Albino Rats We are submitting herewith our laboratory report dated November 12, 1971, prepared in connection with the above study. Very truly yours, --------J. C, Calandra ` President JCC/kjl i DEPOSITION EXHIBIT 35 j'-zr-w NEV 009990 WATER PCB-00051126 >' PROJECT NO' REPORT FILE 1 3ttduUiud Bl O - TEST JaAmata'ueS, Snc. 1810 FRONTAGE ROAD NORTHBROOK, ILLINOIS 60062 REPORT TO ` MONSANTO COMPANY . .. -. *-/ * / . TWO-YEAR CHRONIC ORAL TOXICITY WITH AROCLOR 1260 . >*' IN ALBINO RATS > NOVEMBER 12, 1971 V. 'J ; IBT NO, B7298 . 9 m \ 0q9991 WATER PCB-00051127 $,JUU<ual .B 1 O T E S T jtakvuUMie*, $*tc. REPORT TO . MONSANTO COMPANY TWO-YEAR CHRONIC ORAL TOXICITY WITH AROCLOR 1260 IN ALBINO RATS NOVEMBER 12, 1971 IBT NO. B7298 I, Introduction At the request of Monsanto Company, a two-year chronic oral toxicity study was conducted using albino rats to determine the potential toxicity of Aroclor 1260, Lot No. AK-3. The following report presents the results of this investigation. NBV 009992 WATER_PCB-00051128 * hvLulbual B I O - T E S T /at&iakUU, $nc. 2 O II, Summary A two-year chronic toxicity study was conducted using albino rats led diets containing 1 (T-I), 10 (T-II), or 100 (T-III) ppm Aroclor 1260. Food consumption and body weight gains were not altered at any level of Aroclor 1260 fed. The number of animals dying and the time at which the deaths occurred did not vary among the test and control groups. Hematological and clinical blood chemistry studies conducted after 3, 6, 9, 12, 18, or 24 months did not reveal any affects related to Aroclor 1260. Urine analyses failed to reveal any differences between test and control animals. At sacrifice after 3, 6, or 12 months on test organ weights, organ to body weight and organ to brain weight ratios disclosed several randomly . occurring intergroup differences. The lack of any consistent dose related response and the absence of any deleterious histopathologic change confirm that these differences were not related to the ingestion of Aroclor 1260. At the final sacrifice after 24 months on test, the liver weights and liver to body weight or brain weight ratios were significantly elevated in the rats from the T-III group. Histologic examination of the livers * # from the T-IU group revealed several animals with vacuolar change. This lesion is morphologically indicative of fatty degeneration. Specific fat stains confirmed the presence of fat in these vacuoles. Focal hypertrophy and focal hyperplasia were also found in the livers from animals fed Aroclor 1260. NEV 009993 WATER PCB-00051129 \ D.tduiiiied B I O - T E S T laUmUiiei, Phc. 3 Hyperplasia of the urinary bladder was found in an animal from the control group but not in any of the test animals. The incidences and types of all tumors were about the same in all groups, including the control group, and are considered normal for rats of this age. ' Respectfully submitted, INDUSTRIAL BIO-TEST LABORATORIES, INC. Report prepared by: Philip Smith, B. S. Assistant Toxicologist Rat Toxicity Report approved by: Q Jambs B. Plank Settlor Group Leader Rat Toxicity JaMJ _ Paul L. Wright, Ph. D. Section Head, Toxicology Manager, Toxicology November 12, 1971 lamssjn NEV 009994 WATER PCB-00051130 4' I' Q Q B I O - 1 1 S T laj&urivtiei. $ne. 4 HI. Procedure 4 A. Experimental Animals The animals employed in the test were Charles River strain* albino rats. Four hundred rats (200 males and 200 females) were selected for the experiment, ear-punched with the animal number assigned and housed individually in standard wire-bottomed steel rat cages. Each cage bore a color-coded card identifying the rat with re spect to project number, dose level assignment, individual animal number and sex. B. Organization of Groups A structural outline of the experiment is given in Table I. TABLE I ,, Group TEST MATERIAL: Aroclor 1260 Two-Year Chronic Oral Toxicity Study - Albino Rats ' Outline of Experiment Number of Animals Male Female Dietary Level . . (PPm> __ .......- . Control 50 50 None Administered T-I so 50 ` * ' 1 T-ll 50 50 . 10 T-III SO 50 100 Charles River Breeding Laboratories, North Wilmington, Mass. NEV 009995 WATER PCB-00051131 B I O - T E 5 T XalmatmUA, Ptte. 5 O i i ! i C. Diets, Feeding and Food Consumption . All diets were prepared in the central diet room of this laboratory. The basic ration from which all diets were constructed was a standard, pulverized stock rat ration*. The diet for any given test group was prepared by blending the calculated amount of Aroclor 1260 with a pre-weighed portion of the stock ration in a Hobart mixer. . . Fresh diets were prepared each week and every rat was offered an amount of food sufficient for ad libitum feeding. . Food consumption was recorded for five rats of each sex in every group weekly for the first three months and monthly for the next nine months. Thereafter, periodic spot checks were made. D. Body Weights and Weight Cains Initially, the body weight of each rat in every group was deter mined and recorded. Thereafter, individual weighings were made weekly for the first 13 weeks and monthly thereafter until the conclusion of the investigation. _____ ` _ ____ __ ' ` ____ __ - ' E. Mortality and Reactions ' ;.. . " .. Checks for mortality and abnormal behavioral reactions were .made daily throughout the investigation. ; F. Hematologic Studies and Urine Analyses 1' Blood studies, including determinations of hemoglobin concentra tions, hemotocrit value, erythrocyte count and both total and differential * Purina Rat Chow, Ralston Purina Co., St. Louis, Mo. NEV 009996 WATER PCB-00051132  SnSukiai B I O - T E S T JaS&ia&nled, $ne, i' 6 o leukocyte counts, were conducted upon five males and five females from both the control and 100 ppm groups. . Urine analyses for the presence of glucose, albumin, micro scopic elements, and determinations of pH and specific gravity were con ducted upon urine samples at the same time intervals and from the same animals as those employed for the blood studies. These, studies were conducted after 3, 6, 9, 12, 18, and 24 months of feeding. G. Clinical Blood Chemistry Studies Determinations of blood urea nitrogen concentration (BUN), serum alkaline phosphatase activity (SAP), fasted blood glucose .concen tration and serum glutamic-pyruvic transaminase activity (SGPT) were conducted after 3, 6, 9, 12, 18, and 24 months of feeding upon the same rats as were the routine blood studies. '' H. Pathologic Studies When an animal succumbed during the test period, a gross autopsy was performed. In those cases when postmortem autolysis was not ad- vanced, representative tissues were taken and preserved in ten percent formalin solution for possible future histopathologic study. After 3, 6, and 12 months of testing, five animals of each sex from each group were sacrificed and subjected to complete gross pathologic examinations. i NEV 009997 WATER PCB-00051133 BI O-TE S T Dmc. 7 Absolute organ weights were recorded and organ to body weight and organ to brain weight ratios computed. The following organs were included: liver, kidneys, spleen, gonads, heart and brain. These data were then subjected to statistical analysis. An Analysis of Variance was conducted first and significant effects disclosed by that treatment were further studied by "t"-tests. Complete microscopic examinations were conducted upon the tissues and organs from all control and 100 ppm group rats sacrificed after 3, 6, or 1Z months of testing. The following tissues and organs were included in the examinations: heart, trachea, lungs, liver, pancreas, esophagus, stomach, small intestine (duodenum, jejunum and ileum), caecum, colon, spleen, lymph nodes, kidneys, urinary bladder, gonads, prostate gland, seminal vesicles, uterus, pituitary gland, adrenal glands, salivary glands, thyroid gland, parathyroid glands, skeletal muscle, .. sternum, bone, peripheral nerve, spinal cord and brain (cerebrum, ' *V cerebellum and pons). . The aforementioned tissues were prepared and stained with Hematoxylin-Eosin stain. '` ` . . After two years of feeding, all surviving animals were sacrificed and subjected to complete gross pathologic examination. Tbe absolute weights of the liver, kidneys, spleen, gonads, heart and brain were recorded immediately after sacrifice. NEV 009998 WATER PCB-00051134 ' SiuLtlbual B I O - I E S 1 lalniat&tfai. Hue. 8 Microscopic examinations were conducted upon tissues and organs from selected animals dying during the experiment and upon all animals from the final sacrifice. i, Tissues and organs examined were the same as those previously mentioned. I. Tumor Incidence and Classification A tabulation of the incidence of tumor formation in each group was made at the conclusion of the investigation. In addition, tumor data for individual animals including location, weight, size and pathologic classification were recorded. 9 NEV 009999 WATER PCB-00051135 StuLtikial B ! O - T E S T 2at*ilvUl, Due. 9 O IV. Results A. Body Weights and Weight Gains .' The male and female body weight data are assembled in Table II. The data in this table also include the 3, 12 and 24 month total weight 9 gains. There were no significant effects due to ingestion of the compound Q 4 NEW 010000 WATER PCB-00051136  ; jnudiUAiU^ % % w - q o 9 4J g H oOT' JoS O H <4 >4 0) 6 u -> (SJ M* m m -< fw P4 mm cn *-i m cm M* m ff% ti:) MJ M* cn -i oM* 00 ow "< 60 o O' 00 o6*4 f- eo 00 00 cn>4 CM M< CM M* CM cm O' tn m so mSM C*- o *0 M1 OM' h- O' M CM h- 00 M* CM eo r- M* CM O' mem* O' 00 M* f ^ p4 C'- eo 0N v C'- f- f. M< CM M1 cm M< CM M< fM o o o** r- ^aC O O P*C -d* 0 M< <M m { M< CM x tO cm m> M* cm O' inO sO 'f t* eo cn M< t- M< t- <_t vO M< CM tM cm M* CM 4) *3 m M* o CM * fCM- mm CM 'O M< CM xcn tO M< CM cCn" in vCOM s> 4=C X "5 p m j t.Mv O' m OM* vCOM *o -- M< CM i-^ cn ^ M vCDM cn CM Vcm M cm *o* V 0 0 ,w' vD "4 9s cOn" m cm McOn*' 'mcOm OO O M* VCM0 MOcn*' emo cm W W crn- CinM cm r-n m cm cCwMn m cm m tc~n cinn cm m 4* CM M* %no M< cm --* -x %n0 MCM* eo cm cm Tf cm cn o Vm0 M< cm w O' h* f'- ft "n# m"4 cn cm ec-nC --4 cm cn cm cm eCxMnf oO' -C CmOM O' -c m M< oO' . fM - h- 00 CMM< c "* coCnM n- -4 cOm' XrO 4 -I Me m* o cCM --t o CM cn t^-c- o nn m>*0 *nn x0n nn vcon m cn von W4 eM e=4 n 2 Ui V) o "4 t) o xC0M fc o*? C B >S <--1 u & o3 u 0 r* < A , <*4 N c o r^ SN S fM * o Sh oo .^ ... i NEV OlOOOl WATER PCB-00051137 4* 44 *5 $ fSi T>t c as *3 a| m cb(T) o H 1 f\S oe tj< vm ieng -Or* t0On' ssO <^n m eg sr-o~ emg m eg sOO'' ftOn-' O' 00 j0s. BO tn ^4 (s. 00 eg m eg ts. *=# t'. tn es-s| sC0O0 tt0nn0 e0o3 stssO tn in <-t *tos mtn fs. fs. t0s. itnf a O r- ^ kO %o tn'" to m sso icnn ss0oo 0rtn- _, fsj v0o0 stn* <3 a aVo V 4b1a * V O' 446h1*0 *m-s .. srej<g ionn' tn 0 so m tn to stno tmn 0 n sm ttnn coo o 4) S^.>4CC.04+c3* 00 eegg ir*n< vo tn 0e0g mm so tn s 0 ss mtn seog so tn HO $ l4 3 *8 fr At M tons mn m tn s0O -ten1g 0~0t t<n~i m tn fs. OH s tn . w *8 <* in eg smO etng 0(s0. _T4t* m tn _^ m -- in tn e0mo t0n tf> tn O tinn tn- w t0n +emDg st0n m eg m0 tn tn O^4s rOp-sj S--m0 WeOg' sQ el Oif' O' (SI eemgg Oweg' KV w <0M ^o > *oM - -- .O t:n cu0 U 2I4 a 5$ Q S(N <O~s OC O 2 fa "4 2 fa 0^>4 S fa 00 NEV 010002 WATER PCB-00051138 O ' ' T A B L E 11 continued O' Ml O -i m^ nS tO %n to *M W X tn.^ 0 o m nt --i in m ^m m ns *o m in ^ 00 m -- r** m om t- -* 00 vO %o m in m* X 00 S'- ^ m v oo tn %o m 0*4 in 0*4 e^4o O Mm p- m *x om n> m m ns -< ^ r- w rf rX O r- tn O' pn) n in n- m n ^ tn -< r- tn mm vmO e- tn n to oo t>- m to tm t- m tn tn in O' r- * o K0 to t- m o * in GO r-* o vtO- mfn tn M <- vO SO t" r- --t s> m o 43 x r- p~ * p~ m vO *=N r- m * vD h- c-> t* o 0r-0 ooo m O' m 4) tn P- O' V o S'- tn * t- mrji t- e n vo nr- ^ 4> tn e- to S'. 't 00 TMt 'lO'- 00 tf tn vtO- t^n 0N 'rO '^f m # fn-- # O' \0 m 'O Of n- ^ O vO 'nO- 'O ns 00 o r^ p. m^ <tfp to p. # fsS S'n- <-* t' V O 'O r 0n0 <n 00 ns r vO n^4 -i O ns O' m m n> 4- lh * 0o0 r- to mK> S u* 4 4Ouco4 oo --3 o NEV 010003 U WATER PCB-00051139 $nduibual B 1 O - I E S T JaiotativueS, $ne. 13 B. Food Consumption The data obtained from the food consumption measurements conducted during the first 12 months of feeding are summarized in Table III. These data revealed no significant difference between test and control rats. The periodic checks conducted during the remainder of the investigation also revealed no outstanding differences between test and control animals. . NEW 010004 WATER PCB-00051140 ../ i Jt- d* B I O - T E S T JaJuHaimded, 9*$^, s* o1 U .8 cSj 1m & u (&ft M(h*- ^o t t < Qnc O au ,-v. w yI, pm- 'mO ipn- n n m m I I < *s0 I IQ a Jr ao W 4 B 4p3* I m < H H f-rht! O (coA 0 ooa 1 (*4> }oHt fA ~l O9-4' mpH p- O"4' fTM4 o pa pa mH 0Or04' vO f^s-4j 41 Os_4' mpH pG9-O-4 to re*f4 O' O' O' **4 O' P- O^=4' ^4 *l sO O' o 9-4 o OH' pH CpHO m fH Of"4' mpH to "^*f4 TO pH pH ipnH to O' OpH' pa pH OpH' ipnH N600 pm 41 '9=4 O' tf m M v*OH pH pa Tm^=O4 4< m pH pa mpH N o f--4 0 PO' m pH 00 0% O' pH to4 p4H* pa t*- tpoH o N0 O"4' mM S^ w co ra o pa ra o o pa TppOHa 'O o O<*4' OpH' fTM4 tn esj a> ^0 p- to fO- tpoH TpHO pH eopH N0 o ff-O4 O' 1-4 fsl *i O m PTpOH pH pH o o v0 pa 9--4 o O' OM' I'* PH r- 9-4 IA f=H TO PTpOH opH O' O' spOH tpHo INS H* #TM4 PpH4 (N in 9*4 in pH t~ M %o fA to p H pH mpH O' r*4 ppHa mM <ra o tPoH 5 pH "ptnH* 0pH0 pH ** #=4 ppHa o tn m 0N <* to O' t~ ,CpH-O* in O' n0 4* ^4 O' 0N f4 . 2 fa 2 fa . Sfa 2 fa VT. > PtfK lE 04a2 <8* a oc u o o 14 NEV 010005 WATER PCB-00051141 Srululi'ual BIO-TEST Xa&tMio'Uoi-, Hhc. 15 st*O- ^M 'oOq m--* 'wCM eo M^ 5 (M O 2 <i a . 94 .u8 Ho < *0 w5 (4 <4 Q * C0 1 > fl 1 V 1 i2 SH H| O 0 u 1 H w B H H (4 Jl" fM fw oo cm ># CcMn *o>0m--*> Ow Oeo' o --> Ct"M- fMO* Mso* Om' Weo Om*' O' o e 'O 6N0 NIA vtofi vO 60 visOj M* 4 <-* W t- --< 'ON mm M Ifl O' eft 'O PO *too ttoo O' o C-- r*- -4* O' M* 'O ^ eo tf fM OM' \CoO foO' ^^ 00 "m*< m 'O 'O *n O' <* eo m 00 M* 00 ^ o h- 60 Ml O' ^ oo in oo_ <t*oo O-t' wto or- n cm f* Nh --a *--i hh *0 09 O' ^ sO 00 O' m1 'O P'1 w^ O' 'mO 9 w S f*c S Im Sm S fn *8 S ail> " ^ uJ^ .J2J *?2 oh (oJ O o*- o NEV 010006 WATER PCB-00051142 $*tduil>Ual BIO-TEST jPahyiaiMlei, Httc. 16 C. Mortality and Reactions A frequency distribution of natural deaths occurring during the investigation appears in Table IV. No untoward behavioral reactions were noted among any of the animals employed in the investigation. ' t NV 010007 WATER PCB-00051143 it ttui D 1 O T E S I XaitMaU'ucA; 9nc. *4 tMn M(A uMt Mtn sMjfi Mif# V m O' %o O' o- r AS "* (M h AS -* l mm MM O' M AS AS N AASJI O' M O0A 'O M O' <<f* AS( vO A- O' in<o co m N m 5 2 4d & 03 I %D A- tA a* m r- ^ co n sa & x tI |= A2 m90t*)9 sSJ s Jj .2 ho 02 2 fr ox ^7 at> S & v h OI' - M AS OO ''f M --) AS -* O AS MM OO MM AS O O AS fV=# 5 reoHs 0 1 > s Voo u v dm u m uX V I * 8 *ot O O -HO O AJ fO I oo OO -HO --H O KV m 2h 2 f*i 2 f*4 2h 17 NEV 010008 WATER PCB-00051144 jttdudUial B I O T E S T UmatosuM, Pm. 18 D. Hematologic and Clinical Blood Chemistry Studies Mean male and female hematologic and clinical blood chemistry data are summarized in Tables V through IX. Values for all parameters investigated were within the normal range for the albino rat. No significant differences between test and control values were observed. . NEV 010009 WATER PCB-00051145 9*uLuUMal B i O * T E S T Jahnafotiai, Pnc. 19 o* to t^ o <n K m 2l fcs til aas o bco O o o NEV 010010 WATER PCB-00051146 Dn-Lubual B I O * T E S T labmUuM, 9nc. 20 rv4t 4 l NEV 010011 WATER PCB-00051147 SnduUwd B I U - I fc b I Xatt&iahyuei, 'Jttc. N9 n c-a ea Mo M O' *M O O o SS >0o09 5 J S 5! 2. os ou w i > *uH & O >H W 4 9 I o rt g0) o ffi a o a 3 Ot o m9 'mO e 'O co fO-' froM-e co 00 t- (00" 00 6o0 CO ea %000 n cMo 0A9 w3 fr-J JU '<ooMcw u ,,oO CM n m e < "9* N r~-* oe o IM <M e*H ea e -n* O3' mo 0 n o 'O s vtO'-9 'O 'Oo vmo ern-o <0o*> 'rMt- AMS COn*0 mih- wme %COO9' m CinO oMO9' 2 fc oo 1 * J NEV 010012 WATER PCB-00051148 T A B L E V H continued 24 0.2 0.2 0.2 Sndtuhial BIO-TEST Sue. M't ^pH0 oPH9 * tpoH 00 o o 9 0 pH9 pH0 8*0 0*1 0*1 -3 f--M< g 11 is*u .5 O' poH pH9 w 5^ 5 o .8 %oo 3 MVo. o X o o >us m o w3 a ft > -k No CpHOe tn *H*0 eOH9 S' u 9 1 BO 2 ptf W H pH 0 jj He OV X pH o roo9 p>j oba 6 V fjj #H o9 oo. *rmt II!s>* 11 O' oe o ooe ooo oe eo9 - 00e 00 *0 * o oa o e o o9 0 9 * 'O0 s fa Sex n *2 -- st e V0 H o &co o e 2 fa o o 22 NEV 010013 WATER PCB-00051149 $*tduiU*al BIO-TEST lal&iai&Ual' Pm. o o o o 23 9 3 2 Ui 2h iJ o Co o<*> u NEV 010014 WATER PCB-00051150 HtuLviUial B I O * T E S T JaiotaUtiM, Dtta. s $ o a *0 < 2. u > 3 B ow a > < I wd1 a a1 ^ *a mH ou B fl M4V c 4< 6A -* CM fV6Ol0 _C |a_ * m * U C MS S glia o *8 fot _Mm tf> M< c0 M <0 CO f- ^ w >o wm ^m M $ O M *0 co O n c0o ccoo 2 eo M M M4 rn cMo fVoj in M n o m co ^ co ion co o* ^ co o* c- co o co m <o CO CO wX 2 fo S1I O ft oc u con O' cm 2h oo 24 $ NEV 010015 WATER PCB-00051151 indaUMal BIU I fc S I XateuUoiiei. J/ne. O <n fM 0 a a ra M o. <0 CM CM fM 9 \ i > n fM 8 00 #--4 0 <0 rt m C a *S n tD o ja ^ m fM a ix oc i.. to a o fM O' *1, 0^ r- 4 te to H ffM .a M 0 2 o 1* 8 2 O' in a fM < o "* * 0x a ="4 fM rTM * m & e q 2 s0 x 0 eo X H <M *i o .s VJ ,5 a t<i fM *m o"4 o Q 4) 3H 'O O' aa CO eo SJ eo -< w b m > a z * *H o s 4) a> 1 J3 2 3s H u g *8 0 98 o Xh H % cq rt O8 M* N O' O' O' oTMl to * 00 n tn r-t "4 o jj 1 4> a m 0 sw M "* o o aq CD fM 0M to O' fot u rmt 1 rt o o 10 1rt brt e 0) T 5 C 8 f> O Jj.2 0s o t X5 H *D* u <4 fc*4 CO <0 fM s 00 H a ** CM CM =4 00 o r~ to fM *=# oo 0^ $ &H c m to to H <^0 -t <*0 H S IT Sex 89 115 ,, to 00 fM O to mz4 00 rH s K <Fs &t8 a# o H V 4) a SJ a c o u to o o - 25 NEV 010016 WATER PCB-00051152 SnJudhdai B I O - 1 fc S i lamaUMcS, yc. 26 E. Urine Analyses Mean male and female urine analyses data are summarized in Tables X through XII. Determinations for glucose concentration were negative for all rats at every interval of examination. No' differences were noted between the urine from control and test animals at the intervals of examination. NEV 010017 WATER PCB-00051153 PudtuUial BIO-TEST 2ahyiait>>ue4.. 9no. AS as m fM <* 0< I OAoS < o w *(0 X W oH m mv 4*4 H4 V 3 u .kg 0a 6 J }Ht 1 ts a ce *0 a a * a tn fl aa AS c c oo a a ca aa AS a c aa aa a oO c a aa n c a 6 2 Ik V) ou oe O 00 2 ik oo 27 4 010018 WATER PCB-00051154 ' jnJulfaud B I O T E S T lalmaU'UcS., 9*tc. 28 to to to TO to* t*- to TO TO r- TO a ^ O' TO r- r- r. TO TO to t- t- TO t- 00 C* avt A > 9V 2 fsl + 44 a CO Z X *4 9) mi z1 2 z S - z fc $ * o If z0e Oc m 5^ z 55 Z 1 2 U 4 zto a z 53 2 v 4 n z z fc Sex 100 O 2 fa 2 fa 59E ova S a oc U Zv iys *r O-- rE 5* M II " " W Z *i "I M ft NEV 010019 WATER PCB-00051155 'Jtiduitoitti ttlUMOl xamnamws., y*tc. e>*J C~n1 \ oo o m B OW a 5 el 3 sa 1 W a uH nntK 1 fG H4 ef'Hlj 5 I h vD 0Ha u Vi 2 {* 1 * fO *> CNO fv| ePN*-j PJ I a .. ?1 3WU4O)h 2 m f\nj oo en . O' o~n M" rn 4OfMM O-6' ueM\a0 M*o=01 WO' P'4 EtM* *O0-i K JS S fc o 5 2 6, s jS O *oc O o NEV 010020 WATER PCB-00051156 PnJulUlal B I O - T E S T lalmatMMi, Sne, 30 F. Pathologic Studies Three-Month Sacrifice a. Gross Pathologic Findings No outstanding differences were noted between test and control rats upon gross pathological examination. b. Organ Weight and Organ to Body and Organ to Brain Weight Ratio Data The results of the statistical analyses conducted on absolute organ weights, organ to body weight and organ to brain weight ratios are summarized in Tables XIII through XVIII. Significant differences between a test group and the control group are designated by asterisks following the test values. Organ weights, organ to body weight and organ to brain weight ratios disclosed several randomly occurring intergroup differences. The lack of any consistent dose related response and the absence of any deleterious histopathologic change confirm that these differences were not related to the ingestion of Aroclor 1260. . NEV 010021 WATER PCB-00051157  ftuLtliiial B I O I E 5 I lohyiaivuu, Sne, 31 :'! S ta tis tic a lly s ig n ific a n t d iffe re n ce at the 99 p e rc e n t confidence le v e l. i O 0 o ft NEV 010022 WATER PCB-00051158 ynd4<ilu&l d I u * i co i jcavoviuvucit shc. *<w O & X W J I * *o d u w aj * un u O<T4 *I s eo s Avh I fi 0 to a * 1 |H 0 I 53 +* 2 jtso g 5 w ._. Ui |S^ .*4 **' <4 *> a 'V. V (3 <to4 s U O -1 mm m O' O' fSJ ,rt m O' -l 0 1m 4) *a sN , 0) O 000 o e-4 O' o fSJ 0f.0 e o O' r*-9 m SK 4) C o 2 (3 <4 g " r4 v Mki <4 2 (oMo 4 00 000 o tv. < f O' t*t'-0 o o Bfl m a O' fvl vO 'O f\J m 43 _M E 6 #>4 0 N 9 N f*= *0rx0 A to o f<1 o ttn- oo o o 4 5s a -c o o too | 4(4J OU (t) c o O oo -4 O VU NEV 010023 WATER PCB-00051159 $tuluihial B 1 O I E 5 I Jtab&'iato'uoi, $nc. 0 13 m V M N pH t*- *<3 O fMm e 943 m O' cn \s e SiW e=4 V O o o c* s<4 pH pvj pH t) pH pH m s(to0 rt oe o 0 o e o ot* 33 TE S T M A T E R IA L : A ro c lo r 1260 00 f" <o frv*So tr> m n < m 9 99 OOOo l h 'O SO & V SO "p tm4 o a ea o |v. NfcV 010024 WATER PCB-00051160 DIU* l o l xmmaumm., yna 34 o n w 5 ON e- >s *0 U2 ow K** u O 53 H N U Q 1 w > o j OW H *5 TJ JS I 35 3g > O 2 H * g _. rt 6c0 2 H S M 5 t> i> V 5 o 00 9& M fl rt 1 I & 5m O' NO NO 00 ON vO to M liO v NO 6- mS oooO e ooo V* ^ ,MM 'a4 *? Iutf D # t- o60 ccro- oo 73 3S W) u O t) o o eo On na ('* fO u*> N to M B 0> f.. o o o o o o 03 m n On o "4 NO S'- f- t*" ooo ^ *3 ii < H M Mf="4 n O6 h a S~ M *4 > -3 oNO V <n to r- 2 en n n 1 o O3 . m h B, ts a 5 g'-SI oht 4-1 c 5 o~4 o #2 Q< NV 010025 WATER PCB-00051161  VjtdttiVual diwisji j,,MMnuutsue4., jnc. >? < S o --I O NEV 010026 WATER PCB-00051162 snJ.iii .'jl B I O - T E S T JofourfMUi, $na O n J<Wruit> OTM%*d pVr=>t4 6V t~n) w(M ro n cm co v 1*4 to 3 aw U *3 W .S 1*4 o WV s m fM %f\ * o *A r*- A O 3? M v go ?o OO 60 fM o o O 0s 09 o g en CO 0e 0 oto4 2 o o o o TABLE X V III m ) fM O' O00' e- m oo o o 6 9 M iM c 36 <1 om oo NEV 010027 WATER PCB-00051163 Pnduihial B I O T E S T Ja&Ma&Mei. 9ns. 37 c. Histopathologic Findings Histopathologic examination of tissues and organs taken from all animals from both the control and 100 ppm groups was conducted. Tables XIX and XX list all histopathologic changes noted. All of the lesions noted in the microscopic examina tion of tissues were those of spontaneous disease and are not unusual for the albino rat. The most frequent findings were lesions in the trachea and lungs, indicating chronic murine pneumonia. These oc curred in the control as well as the rats fed Aroclor 1260. i nev 01002a WATER PCB-00051164 HttdiilUUil titO*lfcht Xa^>%a(mici, 'Jnc. I. 38 TABLE XIX TEST MATERIAL: Aroclor 1260 Two-Year Chronic Oral Toxicity Study - Albino Rats Histopathologic Changes ' Three-Month Sacrifice Group: Control Number of Animals Organ Examined Findings 5 Males Trachea Lung Urinary bladder Tracheitis Chronic respiratory disease Hyperplasia 5 Females Lung Chronic respiratory disease Ave rage Incidence Grade 1 1.0 1 3 1 1.0 1.0 1.0 All other tissues and organs were normal histologically. Grading System 0.5* minimal 1.0 = slight 2.0 = mild 3.0 = moderate 4.0= severe 5.0 = extreme O i - . NEV 010029 WATER PCB-00051165 " PttJttihiol B i O - I t b I laimaUMU, Vhc. 39 TABLE XX TEST MATERIALS Aroclor 1260 Two-Year Chronic Oral Toxicity Study - Albino Rats Histopathologic Changes ' Three-Month Sacrifice Group: 100 ppm ' Number of Animals Organ Examined Findings 5 Males Trachea Lung Tracheitis Chronic respiratory disease 5 Females Trachea Lung Kidney Tracheitis ' Chronic respiratory disease Focal lymphoid infiltration Average Incidence Grade 4 1.0 2 1.0 3 2 - 1 1.0 1.0 1.0 All other tissues and organs were normal histologically. Grading System 0.5 = minimal 1.0* slight 2.0 = mild 3.0 = moderate 4.0 = severe 5.0 = extreme O NEV 010030 WATER PCB-00051166 PndMkial tt @ V I t S i Xaimammi, Urn. 40 l I ii i O 2. Six-Month Sacrifice a. Gross Pathologic Findings No outstanding differences were noted between test and control animals. * b. Organ Weight and Organ to Body and Organ to Brain Weight Ratio Data ' The results of the statistical analyses conducted on absolute organ weights, organ to body weight and organ to brain weight ratios are summarized in Tables XXI through XXVI. Organ weights, organ to body weight and organ to brain weight ratios disclosed several randomly occurring intergroup differences. The lack of any consistent dose related response and the absentee of any deleterious histopathologic change confirm that these differences were not related to the ingestion of Aroclor 1260. NEV 010031 WATER PCB-00051167 * S ta tis tic a lly s ig n ific a n t difference a t the 95 percent confidence le ve l. * * S ta tis tic a lly sig n ifica n t d iffe re n ce a t the 99 percent confidence le v e l. D 1 U I t i I Jtab&natvueA, 9mc. o S i2 6O W m s b o j \* 3 2$ PUi j H ^*2 w * Xo 8 H <d-) o o S ao p! o 9 4J JmHS V ffeslf) u a o 4 s I JwJ V B > 9 V s e-i w b e .fc *4 *eM Wb M *; i o a1 a*t0oo a flg*t r- V <co !o* =*# ^ 4? efbpt *V> a * * IoA A * m ai Otbt s s, pa: 3 2rMtmJ hg0 me0 # *>e m tn n o * ft M Ow _ wv * # 0* AJ * O' h- O' tn * a 0 0 e 0 9M 2 ^i fM tn 0* b o Xtoo Va e V n U> *# in V lb s 60 Otboo ** Wd ee oQ O* M 41 t2 b6 o o 4 u =: 0 GO U - o O Q,2 <K NEV 010032 WATER PCB-00051168 $tidjtiVual B I O T E S T * S ta tis tic a lly s ig n ific a n t d iffe re n c e a t the 95 p e rc e n t confidence le v e l. Unc, o9 &3 X4J. g^ s *A*>* *CVmM ^\*4> inM .^M (M 4 tin 8M14 ii s <IM..m-* .m<O--.l'. .O<--' O o ^2 P4 ** e Sal ?> oo S0 WM _ Cno 3125 a*4 s 0 * * *o*tA*** .CVA.OO* .fAlo* Ao*..fo- .r- .mtn V x46>*0 i>2fi mh *55 M$sAi w m Ov 3 2 OtN*-.' mj.(>sj .tmnn .mpan , 9 * A* O^ tfAOe* 000n% n O' 0% 41 > O ao . <M < E Att e2 oO g w c*J o u *4 -* ** .2 ** Q< NEV 010033 WATER PCB-00051169 ^ I * I b # JQUi. -a^ S ta tis tic a lly s ig n ific a n t d iffe re n ce at the 95 p e rce n t confidence le ve l. V OM o *4 QVf<z4r^ wO ` HbhOUo < EffC>t],| C o O # nev 010034 WATER PCB-00051170 * S ta tis tic a lly s ig n ific a n t d iffe re n c e a t the 95 p e rc e n t confidence le v e l. <f4wai'nnuu> m w i ^ @ I. io ^m.. 44 * wO' o o tn fNsOs o o o NO or>9 & roo o r m r-4 r~4 Or-' tO-' 00 o f* foNej \J 04 O o oooo n Om' 0 NOn NO d o M NO 0 NoOo NO o oo o o N o 00 NO * o oO' M O' ro- o0 0 o 0 o mm 04> ^0 n6A tmiao o g # ro* o o " U NEV 010035 WATER PCB-00051171 * * S ta tis tic a lly s ig n ific a n t d iffe re n ce a t the 99 p e rc e n t confidence level. yadiUl-uatr BIU teal xam%awue4., yme. O I55? 56 0 in o n meo o \0 o o o 4* M3 in o a ^h |s^ tiO ! .m a s a s mU w<o o <O' o o*o* O' 41 t- 5O I * K O A 4) B fM Oen * o rrw o r o n O 5 \V n o s a,./ m u fl o 3<4 P$ V 9 o u euP4 V A H <4 6 0 44&VHSAs oc * 2 is * Vt sffi > feMo \0 eo m CO 03 fM fMo fM fM e 1 O O O o * w> O <$ 1 9w W) 4 fl <5 a a mo tm-i m <o oo N ft B a a I &t w> a oa *3 m r S 45 < 3 faM - M I* C ooa *<a4 rOo2-t wQ, oho* 6 o-- oo wev 010036 WATER PCB-00051172 O 5 6 I o mB * c ToJ H a 5 fl 4>t e i ;' / TEST M A T E R IA L: A ro c lo r 1260 * S ta tis tic a lly sig n ifica n t d iffe re n ce at the 95 percent confidence level. NEV 010037 WATER PCB-00051173 ; V $ivinlt\ial B I O T E S I la&MaUtdM, 9m. 47 o c. Histopathologic Findings ' Histopathologic examination of tissues and organs taken from all animals from both the control and 100 ppm groups was conducted. * Tables XXVII and XXVIII list all histopathologic changes noted. All of the lesions noted in the microscopic examination of tissues were those of spontaneous disease and are not unusual for the albino rat. The most frequent findings were lesions in the trachea and lungs, indicating chronic murine pneumonia. These occurred in the control as well as the rats fed Aroclor 1260. 4 o NEV 01003a WATER PCB-00051174 Sfjulkld B I O - T E S I laUtaiMded, 'Jne. 48 TABLE XXVII TEST MATERIAL: Arcelor 1260 Two-Year Chronic Oral Toxicity Study - Albino Rats Histopathologic Changes Six-Month Sacrifice '' Group: Control Number of Animals Organ Examined Findings Average Incidence Grade 5 Males Trachea Lung Liver Skeletal muscle Tracheitis Focal tracheitis Focal pneumonitis Hyperemia Focal pericholangitis Focal inflammation 2 2 1 2 1 1 1.5 1.0 0.5 1.0 1.0 1.0 5 Females Trachea Lung Liver Kidney Focal tracheitis Hyperemia Hyperemia Pericholangitis Focal inflammation 1 . 1.0 2 2.5 1 1.0 1 0.5 I 1.0 All other tissues and organs were normal histologically. Grading System 0.5 minimal . 1.0 * slight r~ ' 2.0' mild '. 3.0 * moderate 4.0 = severe 5.0 * extreme O NEV 010039 WATER PCB-00051175 o - 9 .. j i xaw-vmvuc*. j/hc. TABLE XXVIII TEST MATERIAL: Aroclor 1260 Two-Year Chronic Oral Toxicity Study - Albino Rats Histopathologic Changes Six-Month Sacrifice ' Group: 100 ppm . Number of Animals Organ Examined Findings Ave rage Incidence Grade 5 Males Trachea Lung Liver Tracheitis Focal tracheitis Focal pneumonitis Hyperemia Hyperemia Focal pericholangitis 2 1 4 4 1 1. 2.0 0.5 1.0 1.5 1.0 0.5 5 Females Trachea Lung Liver Kidney Focal tracheitis Focal pneumonitis Hyperemia Hyperemia Focal pericholangitis Focal nephritis 2 0. 5 2 ' 1.0 1 3.0 2 1.5 1 0.5 3 0.5 All other tissues and organs were normal histologically. Grading System 0,5 = minimal 1.0 = slight 2.0 = mild 3.0 = moderate 4.0= severe 5.0 = extreme NEW 010040 WATER PCB-00051176 * PmAu-lUkd B I O - T E S T JaSmaUidei, c. SO 3. Twelve-Month Sacrifice ' * Gross Pathologic Findings Gross pathologic findings among test animals were not significantly different from those noted in control animals. b. Organ Weight and Ratio Data The mean organ weight and ratio data collected at the twelve month sacrifice are presented in Tables XXIX through XXXIV. Statistically significant differences are designated by asterisks following the test group value. ' Organ weights, organ to body weight and organ to brain weight ratios disclosed several randomly occurring intergroup differences. The lack of any consistent dose related response and the absence of any deleterious histopathologic change confirm that these differences were not related to the ingestion of Aroclor 1260. " O NV 010041 WATER PCB-00051177 * * S ta tis tic a lly s ig n ific a n t d iffe re n ce at the 99 percent confidence le ve l WATER PCB-00051178 * * S ta tis tic a lly s ig n ific a n t d iffe re n ce a t the 99 p e rce n t confidence le v e l. MjattltlUH D I W l i. J I jLuO^tuumv.t, /tic. Q 2 (5 o JSo <4 04 OS cn mO' m OcO' 6J) 47 ^M S ^ <it4 V47) o9Mto a 2 Or"4' o CM C"M# 0f*O0 2 CO ?' <rt'n- m trn ac4sa** * 9xo H s -rt O u Aa0uid U #u 9W{tVr=otd 5 g0 21 <t>7 41 VI JS O IS o V | > %47 2 v> 47> *0 2 vfb4o *^7ta? (to o -t o to M .4G* = o ve4) tr C <h4 S44 t22 oG<46440 w Oc<M' cmCM voOo omo h4 V *O1 * H ja mW47 n V**I fM # rC-O M oMoo ss w oto V4)I a 2 oVo m tn O o <^t m VV>- Vo G Tiv4J47 Cou * G Vo|4 4O7 t n O' 47 5 47 V G 7 It 3 o 4^ 9 (7 s & 4477 1E S-S Q4e) o It GO U o * O U <4 V) WATER_PCB-00051179 I i JS o< 3 I as o u -4 oh 8< X w *1 9W H Ha Vi (v4 0 NEV 010044 WATER PCB-00051180 SttUiOrum v/ i & i i /4<C, r*- rin- m eino ea in o . # O0 o. ooO W 43 wu H im d 4) OI oe- fwsS O' 0 0e>00 mt* m t- r- 09 'f 00 O' *n 3 f\J <\9 CM OOoO 2 MbHo <__sb^e B V Ui o . o e o 0 o <4 o * a ** 43 t0>0J) V : o O 8ub> o w> w 0V) g mu s O 10 O' A 0 O m IA 0 o eo tm- # CO O' 0 o *o gfbeO o * S ta tis tic a lly s ig n ific a n t d iffe re n c e a t the 95 p e rce n t confidence le v e l. * S ta tis tic a lly sig n ifica n t d iffe re n ce at the 99 p e rce n t confidence le v e l. *ouco* U O o -* o WATER_PCB-00051181 o 5 43 o ao s 5 Mt 14 O o*4 W * aFVutudl < uA Ko H *0c 3 O 2o1> o**4 is*) a 5 4J tS tf 9 IS m v0 > S 4) s o frct* 9H 8 oBll xt V bue w O Hu ud o j t r- N03 nO Ort n o ooo *On' f^ <--3 \0 1A*. \80 M9 rM9 M9 oooO 4 oo NEV 010046 WATER PCB-00051182  Valued B S O - 1 E S 1 dah^uda^ici, Dttc. Otn' min meon ea een' 0i0f>0* o o mr 56 TE S T M A T E R IA L : A ro c lo r 1260 $ & Vu o US <4 o *4 & S <0 * 0C 1Xwml s( * > 9 BO <$ <0 PS V> a ovo 0* m<sj On' n 0* o> 5 \x ee> 'S Mh 1^0 .s 0 ffl l-o5"Cw> l^ rt BO sTMmu -Rl O' 0**> O0* n 5O eo m o *3 * fi Mo 8 CO o O' " V ^M 60 k> o --*v<J0< 2 3 fa0 to in C#O- fM 5 r-1> o 0*tVS3t0 ou "4Uh8> 00, O' O' V A V h 5n u ou Ios O * oo NfcV 0i00<%? WATER PCB-00051183 c. Histopathologic Findings Histopathologic examination of tissues taken from each rat sacrificed from the control and 100 ppm groups after twelve months of testing was conducted. Tables XXXV and XXXVI list all hisopathologic changes noted. All of the lesions noted in the microscopic examination of tissues were those of spontaneous disease and are not unusual for the albino rat. The most frequent findings were lesions in the trachea and lungs, indicating chronic murine pneumonia. These occurred in the control' as well as the rats fed Aroclor 1260. 4 NEV 01004b WATER PCB-00051184 90 9 TABLE XXXV TEST MATERIALS Aroclor 1260 Two-Year Chronic Oral Toxicity Study - Albino Rats Histopathologic Changes Twelve-Month Sacrifice Group: Control Number of Animals 5 Males 5 Females Organ Examined Trachea Lung Urinary Bladder Trachea Lung Colon Findings Incidence Average Grade Tracheitis Chronic respiratory disease Calculus l 2 1 1.0 1.0 1.0 Tracheitis Chronic respiratory disease Parasites 1 0 I 1. 1.0 1.0 1.0 - All other tissues and organs were normal histologically. Grading System 0.5 * minimal 1.0 slight 2.0 s mild 3.0 * moderate 4.0 > severe 5.0 extreme NEV 010049 WATER PCB-00051185 $tulniUidl B I O T E 8 I JoUmh-um, 'Jhc. sv TABLE XXXVI TEST MATERIAL? Aroclor 1260 Two-Year Chronic Oral Toxicity Study * Albino Rats Histopathologic Changes Twelve-Month Sacrifice Group: 100 ppm Number of Animals 5 Males 5 Females Organ Examined Trachea Lung Kidney Liver Trachea Lung Findings Incidence Tracheitis Chronic respiratory disease Focal lymphoid infiltration Vacuolar change of random cells 1 3 1 1 Tracheitis Chronic respiratory disease 1' 1 Average Grade 1.0 1.0 1.0 1.0 1.0 ' 1.0 All other tissues and organs were normal histologically. Grading System 0,5= minimal 1.0 = slight 2.0 mild 3.0 * moderate 4.0 severe 5.0 extreme . - O NEV 010050 WATER PCB-00051186 .PtuLultiiol B I O - T E 5 T Sac. 60 4. Final Sacrifice ft. Gross Pathologic Findings Gross pathologic findings among test animals were not significantly different from those noted in control animals. b. Organ Weight and Ratio Data . The mean organ weight and ratio data collected at the final sacrifice are presented in Tables XXXVII through XLII. Statistically significant differences are designated by asterisks following the test group value. Absolute liver weights and liver to body weight or liver to brain weight ratios were significantly elevated in those rats fed 100 ppm Aroclor 1260. Other organ weights, organ to body weight and organ to brain weight ratios disclosed several randomly occurring intergroup differences. The lack of any consistent dose related response and the absence of any - deleterious histopathologic change confirm that these differences were not related to the ingestion of Aroclor 1260 . NEV 010051 WATER PCB-00051187 DtululVUal B I O - T E S I Jai&mUtuS, Pne. <4 o4 ** X em=4 ti)l M E0 d* .40 (x IM %toom %PO'DSO' <opos03 0*4 V ^ (3 m r2Nt ^w60 "fi t <4 W M ^s| <4 O2 * n o o O' pa <r O' f~i 61 & 43 O n (4 m *0-4 m (0 E o m m n m O' 0-4 n # pa =4* 4J 0 5 * a f) d m (>4 t* S o v 5 <u *3i a 5 5 w 4o3 d 40 Is rt _ 2 %sj > VH a 4 u <4 W M 0 a t O DO -- cm <4 0 o * * r H 5 J6H30 0 o X f4 IS .5 M IVi <4 60 m H 5 O wj 2 0 n 0 to eo 0 r^l 'O e 'I* ue e*a 0 *4 <4 &o M o >4 * 1 o m m*) n 'O am * # e 8 0 'O o M 43 >MH 0 In _ 5 60 4 w M 6 m 0=v4 <4 2 rMa rfa'l r*J #* O' OC'l' 8 h O a* M So3 ~ 2 o o U V 4-4 <--1 V0 OO cc V0 *0 Tjps=-t#j (oS CoS uu + *J Vc tVt ou >04 H0 aa n O' O' O' 00 55 44 44 <4 <4 00 uo (3 a 00 >4 M j> A aa ^*0=4 40 s<&s <&J au au =4 eCm^4 C a (=! nm 44x*-44 e-s-*44. <U4 U4 aa m #N m aa tn tn !! 4 4 NEV 010052 WATER PCB-00051188 . .. .4 U I W 6 I. J I O.tMMfi'MdmM!*, SHG. Om (4 *s Mm rt E > J O O N <*> eo M '* O tn bt .5 " 23 % efl *< --mt At o 8A M n 4 o tn Q o o "<r 0 o 2ooOo o a At ci 4J E V A imV4 ' tofl m* T^O *^4| 40 oo oo Vu c >- a ss ud W 4 a 3 w 0 "c At es f--Vrt fM ' TO 0~40 --# e *t tn-4 CO tn * o.s efi 4 O soooO I OJ 4 2 H* 30a, n o on U oo NEV 010053 WATER PCB-00051189 o o* m m m (0 o e*-a m J3 6*0 \G 6 t> o oQ t- O' ut o S> CfN 0 Mm >*, cm * d M Wi>>H !A %o tn m tn N Q0e o s 4 =# ** my 010054 WATER PCB-00051190  jeUU4il/t44J4s U I w * i 9 <d*U44-. oH (5 44vot2J*o wV IS 6V l* (0fts fo fssf- ro OS 6O0 o o <t< sr- o .S " i3 ffl "e <mu4 O V4>) flJ s vo0O0e o 0os0 o w oo o oa* # o t>t> < NtV 010055 WATER PCB-00051191 SitddtUiial B I O T E S T lahyialtMici, Due. m o jj ,, *s Si! 60 nt 7E imn mmnt 3w 5o * Jm ^M PE< g c3-S.8rt ess AS * vO d* IA * m m eTM4 d* V m 2 o .8 3 n--si J* m d(4 ns l*. r- CO v o e' tt >O4 S*N Uo. w5 o *U It V Ant > X fu9 t< V 5 V a 1 S. * oH M 30 0u) mSor-t r-j .s U* Am ^ . .nu8t a e n 40 ufGtf O (Q fd w nV WMnt) d 2 o en Adn*) dmM*6 n Iin#*rfsv)9 en $n o '0 o n6ct0 f-4 O 0 um tNv mO' dO*' sO O' m O' 1 o is !MS OU m) *d s 00 AS ns m--) fMs m0 3ns0 o* a? 1 24> Ou c U -4 o o o 66 NEV 010056 WATER PCB-00051192 $nJh<iti*al B l O - T E S T la/makvUci, Shc. 67 c. Histopathologic Findings Histopathologic examination of tissues and organs taken from all animals sacrificed after 24 months on test was conducted. Tables XLHI through XLVI list all histopathologic changes noted.' Table XLVII contains the results of the histopathologic examination of the urinary bladders. Significant liver injury was found in animals fed 100 ppm Aroclor 1260 (T-III). The compound associated lesions consisted of vacuolar change, focal hypertrophy and focal hyperplasia. In addition, there were lesions of inflammation, necrosis, fibrosis and minor degeneration in this group which, although seen in the controls and lower test groups, were more severe and frequent in the T-III group. The vacuolar change was not seen in the control animals but was observed occasionally in livers from T-I (1 ppm) and T-II (10 ppm) _ animals. It was frequent in the T-III animals. This lesion is morphologically indicative of fatty degeneration. Formalin-frozen sections of livers from ^ yepresenafcive animals which displayed vacuolar changes were stained with ' Oil Red 0 to reveal the presence of fat. The vacuolar lesion in the cytoplasm of these cells was positively identified as fat. The hypertrophic change found in the liver was focal and often limited to the central lobular area where groups of cells were swollen to two or three times their normal size with clear pink homogenous cytoplasm. The hyperplasia was associated with the same cells and appeared to be an ' NfcV 010057 WATER PCB-00051193 $*uLtiU*al B I O - T E S T lalMat&'Uci., $nc, 68 extension of the hypertrophic lesion. The hyperplastic cells were also usually hypertrophic. The most severe examples of hyperplasia appeared as nodular growths with limited compression of the surrounding normal hepatic tissue. * The minor lesions of degeneration, hepatitis, ductule cell proliferation, necrosis and focal lymphoid infiltration seen in the control animals and the T-I and T-Il groups are lesions of spontaneous disease and are not related to the Aroclor 1260. This level of liver disease is not unusual in old animals. Hyperplasia of the urinary bladder was found in an animal from the control group. This finding was not present in any of the rats fed Aroclor 1260. All of the other lesions in other tissues found in these animals are related to spontaneous disease and they are not unusual for old rats. Donovan E. Gordon, D. V. M. , Ph. D. Diplomat, American College of Veterinary Pathologists NEV 010056 WATER PCB-00051194 o . jew*. OV & f5| t> ^ <$ oooooooooooooooo o e o s (nO'HNH(n(OMNHHrttHN u a 4> n b m (d SB a g-sX S fl o au^4o ug eOo=4 ,W53 f-4 id H & to 4=9 o a u e a o*p< O *41 0H1 t *.so .s to H (4 oU fi 3 g o O X' o< Co L) *Id; *H N av wc o 41 <utf 4f0=H*4) 4*= mw *2 mH ts XM 6 s, " w a^ ffic$S N c rnt H V Uh 4*2> *g* g 3 .y p N id es .COC< fOrgd P^Igj OhQ g 2 js u o S v a o U 43 O si w _ H ft id VI V) i"s *mH> js g eH> Wc> id s frj-s xa u x 4ag3 4.H3 -r3t ,2 3 ' vr*t -l iogd H 2; U* id 4CjJ 4vo3 oa tpj, id id C > o k p .5 g X m 6ss5 10 <0 a H .9 4# UX mw 0) *o4 d #4 NEV 010059 WATER PCB-00051195 Unduibucd BIO-TEST Ja^&Aaifuded: Due, 70 t) r6Ut0 "rvot vu OOOOOOIAOOOO f\J pa* p** w* ) *TM4 tap* ^ p< | pa* pa* twl |o^Joeop* opa* (op* opa,, opa, s & I S< 2 m o -o 4fe)O u2 s5 w r u uV o u o Xo H 3 5 &o uo $ o i3 Hrt *mocw .s a g O (4 o ao tHn a a Mrvt o< u rHavou r>. n *=i n w m -i <<' ff* s *i O" -<t* -i s V) if & s 6 I rt V aa Mi Trach Lung L ive r C o lo n Spleen U te ru s O va ry A d re n JOr4 ws rt *u3. tn w tn ruWt &2 JrS 3Sy "XCMpUroHt M-m>> .Ma v (md V e o>4 X o < a a .S o u o H a U 0 *0 S $0 *8 d IT 1 0> m4* 2 'i in a du to ** *c o > i> <0 to t ti i oc 8*3 <* u 01 N u <* s * wW Crt MC g ffsg II , o{ T3 O fS3 f V4 <0 rt |g l< m vmr*4t tEVn NEV 010060 rt H M eH '. V X4J E' o a \f\ c < WATER_PCB-00051196  t> s z"o r OOOOOOOOOOOOOOO 9^'9eoeee u c v *a ^C^^r^^fS|eM<*rtetf,,'r*4 f\| --J 5 I 9Bu o X w w> *3 om B *4 3 if 6 u o rt t* 1 ss ,,o60 y rt a H *3 W S a a, S*fH sd .1 SO s*y t 44 fet m O a 0o ss N d o o W (4 om H *o pct a T3 rMt U O X ow *>l +4-! o * dolh-i xrot 6H n -) O X. 4ho4 <fe4 m m a'-g 0ft>) d CMH U OOS U u a (4 V U B fH m '2m uc <4 8o 6 O U< Ui ffi V JJ <4 gIN *H O *{ a <n ^ h <4 5oo m o **O-i rot g xfonUcij uoP5G. U < ffi g '43 (4 V 0 -i-i 60 H*6 .2 c 3 u *2 60 -cOW .H2 cO r^C OOH rt *4 4-> M H _4 & Co fl rt rt Q .5 fol -fl rt rt *3 .5 <4 6 * 0 *0 v (4 W M 'S 00 S c Mrt.l rt rmt Cp .>5 IHJ4 u O l <4 C 43 X > y G ! 3 i|5 & o f4 0. Sem inal V e sicle 4 rt 2 NEV 010061 WATER PCB-00051197 v t> > *5 2 g oo OOOOOOiAOOOO O r M m4 nH O fVJ P=l pa* T A B L E X L IV continued A c a n th o s is 2 & O & 9 x o m 4> 2 to 5w 4) U 6JHr a u 1 H --OoMl VOt rt W rut O o *<Of*4t .9 m a o ffait ft g 8 H HV I o V t) c 4) *eu0H P"f 0^* eH TM3 M p"H p4 eH fSj 5 oh> V) 7ff5*t fsGt>o gH* ga V 'g o CH Sx X vt 43 AS P rt s8 V f> W aH *H *o *0 Vroti M <ot oo 3 X X 86 not rot c 'S5 .2 t*oH OH W oG Bo 4o3 Vi M (it 43 43 M UUH wrt wV S X 4VoJl rt OuH _v) *ft'S2 LWO 4gV3i oh ^ a o-4 o nt 4V3i OO U Ui oa art uij rt m.S orf-tit O Vi 43 V ft ft rH O -< (oit 4uJ SS .8 V 60 c o O 4 43 .2 scntpo-uwa * reto Jo3 G PO u rt J3 >u *o e n"=t* o 2d W c V g u T3 be < Vi a 4=8 u t O 60 (it e Vl p Vt 9) J! a h (4 m o pr=Ht i 2 # NEV 010062 WATER PCB-00051198 t 4 ooooooooooo u c V *0 *"! ^ c*4 5 px, 0* T A B L E X L IV continued S< S3 o 'H n0bO aS S--6ooI0 3 rOt, o a, a ,.sCi O ort 5rurustt (mV"2*mCmoW0erot{l ku3ov6coOR>0 JO3tfCocaAJ4tl 4>o6crCrO3tt0l SH..a-o6crO2gHt02'M,'*g_dmgscr^o0t,i*Uf*o?06COl!0 s rt fi E V0 w2 O.ci wa. *8 *a o 6^ 2 o S#*4 o 25 D< e> 13 6o Ui NEV 010U63 s a*(yt4i-a* o V c0i .56 > *Uj Vm vH *fWo4 ii it oo JA ^ in o R 0 >4 E wCol <M <n o 8 D V g m .3 X c .5 .? V E *5 o i ii tn o WATER PCB-00051199 ?1 oo oooo oooo it ooo > VCOt) MNinHN-<Ni?veNi-< n e ^ -Y e a r C hronic O ra l T o xicity Study - A lbino Rats mmv a <4 8 a g a 9MOO-4 O W 2 .. a.rS s $ o in 6 a OmDJ .TB5r3* w VT*#=># to <t>4 to <v <0U>4, oXk ^6 (4 A rt a s haoHo y<Mc4 o qoM o^6 *U A(u4> rVt <4* 6ac9 SH'J 3 8 OB MW I o 4> . . e ^ rt 2 JT8Xjv4<r*t mH0 TS4M3) w * 6 <5 4JJ* J<VU34 (V4 U(4 GC ffi H ^ --mv4 8* <4 sE 2 li V D Jn NEV 01006^ WATER_PCB-00051200 UnhuUial BIO-TEST Xab&iahvucl, 9h. > V "1 1 oo*oooooooooo 75 T A B LE X L V continued 6 V c Oort -4 9*4 p-4 H pH fNl O !*" pH t*-- p-4 r=4 soO ehOuo-t m 6v0 6 Moo=vHH vo uuH W H 3s s. 4o** S VI H a a. .. Cti 5 fl s S. W d MU C CO n ao to g. (4 XO s H O 8 rt > W Oi H& & *** H 3 O to & 8" oVHi ?XVVat 5 *c S si C u S oI2 o ^ ravvt og8aw oxp'3vht _8nH ULM, ofi 3o jq H^ & rt " B d ^ -8 Ow wtl wo 4owaH- o wcoto uft<;su2uhzu n 4$ fr* Vi 6) > uvo B vJ{ Sq SM S ,*rJt S2 63Cg3g 5 U!2 B ^ 4j w w y ? M o# f* E 41 to NEV 010065 Sk S*Ut44 I 60 TMO| $ Q> 4o-> rt St oo A 4 tA o ti 4V8>)t * 4V 46t>4 n T> rA g .2 5 ii ii o6Vt0 eHc0d o fsi in 0 0c5 (M8 O V p Vt 4) .3 x- epCH t/ 5 w O Ii ll tn o o# -- WATER PCB-00051201 o ! i t vv s S OOOOOOOOOO OOOOOO (M *H ) *H H (M Iw 4) c V "0 tft(80'i-NHrtNHNpjfvj(v,HH u H em osiderosis Focal lym phoid in filtra tio n C alcified concretions in pelvis V n n nl a ^3 -1a-4 M o V .6 w ^O 4~3 OC ' tu 4) & 4HJ nS V 4 ua bx .s sf*t 38VOo4 .M y .H oa 5o M 4 6h 4) .a BfiO <H4 (X t4 4) <0 4) h_ B4aO) O b J5 *a o 4) D -4 W> 3 S MCOO ji o i o UU>h .C H nl <- Cp o ,fi *n o2 BcO JcJ O 4) UO > wa h to nS oa a 8 u .21 bo O* a s V ,fl HO5 5 0 < Vts 1 <4 ft W 4) N U 68 H 4) i <4 <M4 C3 SHJ fc a* f=4H) <4 2 o S p le e n K idney 3* 28 *S8 2B &$ NEV 010066 WATER PCB-00051202 es e ct9<Ajn 77 m <u4 o t> 3 O O O oo o oooooo Vo cv oopo^i h -4 h ef) 43 W fX> --4 m* U" V acuolar change (fatty) T A B L E X L V I continued t*>>o sS g u aa. f6Ot0 o wn) oo o ft flj a rai .8 u oO w > 1 H 8 4 * JVH I *0 .8 f=J LJ "=l 3 30-133 &S-So o 3g o c oe 3 . >* *> *d g2 *23 ^<SS w> okm 6>.0* ">g04 K h ftiH < # to m Vrt rmi (fV4ll o o X o aoo a foi 5 2o oB ) 6 O a o 7m3 rt S>6 J.t3-t CO T130 OHoow 4 + 5 dm (u3 gm L ive r O > m *3 &f-o4> 6 NEV 010067 s m I WATER PCB-00051203 V 2" 1 ooooo If em4 -4 f\| | oooooooo 3| gs H tj mv 60 s ao0> a sH6Oo0 <VuHl wrt 04 o o tS la .art a 64WWoJ (n a V "Oud0> IA fM *0 CO h H H H H ntHo a) s3<a? XgN H 5 r* y 8a j9bmcHd fiCH Vr0<)i a) 10 B fl) E a h c<}a c z -a id O oy 4m3 hU 43 V<* u V a 43 Vi #i3Hd 'O , VH) ow Vawi gVui vo O 5 .S o gOa, rxHaH j* o H .2 J22 o> a g2 *W0 6 a 2 x g 2 g rat, a pH 8 a fl) 3 >oo* rfyo{l) id * ' ^ ao 3+* -eo 2 8 H Xo2 `wfHl) mrt V?l W 43 nr(1t) a Vi y o U e> !g m q a V C y2 Tl St c o 1fc0J o 4f*l) a >, c u J0 H Vi b> id oH(U0 a id (H0 fl) X In B Vi tj C h #43 5 O SU^Uh SC a i urt 60 *"oTMl o m 4 H3 o & 0%) IV u .a c o 1u s 3w Vi V > ff m *04 fl) G V h m 1 28 aS }fK 3> *I1II TMfi -.5 3 8 2 | l flsassS NEV 010068 O (3 >` Vi So V) fl) M 60 V &o *o c 9 3 *>a XI Vi V 43 WATER PCB-00051204  O Mrt ) *<VMo4 <mocVv u *H C^| I A TABLE X LV II o 4> S o^ <X> < N-t n x .50 $ rt *3 o 5 to h sV o *oa V o H erh*Ht MV trot 60 o .s o kt co o f6=*0 6 -o3 M3 tfl rat }h o 4= V H W toe*--i M v a IA O V) rt S &#m VJ- v '0O MC l W& 60 5Pt kt W H gv uV rt rt .9 V a wpui o kt 4> V .9 &S no eo 5 a V30u 1 o Va 1 t'- 60 a ort .9 3o oa uo At a -H T* o -* r 'f* o * t8o 2 to 2 k -2 kt 2 En r Sm O O 8 Oa -* Oa H C. i t_j M< M IO Hw I a, o| H3 H N to NV 010069 WATER PCB-00051205 . yndMU'tMH j,uvuuo^ts4., jnc. G. Detailed Description of Tumor Findings Tumor data for individual animals including location, weight and pathologic classification are presented in Tables XLVIII through LI. None of these tumors could be related to the ingestion of Aroclor i 1Z60 and are considered normal for a random population of rats this age. f i ! 4 i X $ i NEV 010070 WATER PCB-00051206 ^M M M r- M. IM IM im d* ^ M IM SJ da d oB 8t> .do004 'O8w 4odM3 d o d du> u , du d s S B 6d o < 2 2 Pi MB 1 $ CJ INJ ^4 0 KX e-S fM t XX m fM KX co m XX M IM d B d Bo ocOV d a V rrtr Md ob s E H d {*4 4* K K n 13,x 11 x ,4 230.00. . Abdomen 4M5 n K M 0 CO O' r- ^ o --4 sd& ff%A OM' 0 CTOO s tvS 'r*j* 68 ov 4*03 *U0 << Oc 4Boo < NEV 01U071 i 2 t*4 rvgj 'O ut* tt f 00 r Int 1*14 o fM r ' %n fO*44' %CS 1*t4 t vO 66-F WATER_PCB-00051207 M ^aw g o M (M N N tf* M fM (MM sH e4 s TRv3 V |-S <4 2 0 0A I 8 8 51 a* o %fSa| 0 nW I &O 5 3 w o UO I 1o' O rt oS U A os X ua o w p 9 H o H O *3 M o o 0 o 43 Li O fr, 0C SNHA wRO KX t <f) 8 sO XX *oa JJ ot0o lf Up e(4 o *Rv 5 P4 K. -n* K n \u <4 0 1 *(M) w iS I toors0 N 1 *0oD0 Mtoo~. 1 " I tCO-O*l8' moootf0 a t; 3 is 3(4 s a G 0 $*8 q >, 0N RR 00 B 4E E 4* fr 8 6 8 3-8 .-8 3 <4 n < a3 3a o 3 O NEV 010072 Sg ws u 55 s1 O' #Ur\-1ii \rmi. ,%:* ^tUn10i Uii f#mU*N1#i fcmU=M--i4i WATER PCB-00051208 ! O' dw Mg0H* # <\s <-4M* "<NtJ fsj fM fM *. M a m m a ry fib ro a d e n o m a w oa io 3x 5x 2 s I i *b>O iT wB 4.9< pI *rt o a a o H o rMt y o(3 XPJ< oU U a o oWc 05 u <v4 1 d *V0 <4 V 8 *004 1 M vc SB W X 9A X 4630 b Ml oooe O' du 9 to K n K 00 0 !t*n 0N 5 u *8 & Sd *4 a Ctlt Bo <o K( 1 a 9M> 'Vao 3 1 4M3 u EB a ^a 4 ?4 1 od a '& is to 2 9 .0 Abdomen b 1 '5^g 54S. Tdd) eum\9s* Ik 6fOM3i uI* N *pM(*mo14 ft* NOfM1 Uti fMM NEV 010073 WATER PCB-00051209 <^#$4441 O) o'l 5 od s do y H fM of 3 05 I 5 WM od rut a*(9H0) <0 6 fI *0 1 wE OM ft ou 1 w H aW t-SJ o u O ft do fUt O V WN**4 X eo K o O *QvuwC *0 HaV JHD e E X 2, *^ o vIoAD9 sn X ^ X feO4ao9 <4 oc rout *4 o>4 Sc ^ .2 sr >UN 2 1 ffi g: Eo .t^Oj oSoa(4 ,1 5 .yfi wXy co NX .ffMM <* cn1 fM -SMA0t NEV 010074 WATER PCB-00051210 /< \ u o v-- " l. s i xawwimtM, yne. O0 mv H ^ C8* fM fM ^ en M cm . ea ran I i ! 9 TEST M A T E R IA L : A ro d o r 1260 00 V0u %dmm m 0, .g is VOi ! a* oo O C0 UHUa g01 s 3S) E 2 Si ^o itn- nn e mo a 8 dwVMO0 && Vi V> > 2 shh e lf # 4* M* vO eo O' O' m fM ' fM fM M Ui r O 01 NfcV 010075 WATER PCB-00051211 "t * fvl iM M f\*t *0 I JJ Poy a W 1 5 H 34 I 3 n W fI m &HU O 1H H -* o In o oa y 02 y il w V OQ u <t>4 !*1 4 6 o a V <4 o s <4 O Sirt u 8 <4 H P< aV B 'a* 0 ! *4 43 u \ E1 gg VV *0 <4 (4 0o fMt fUt *9 *9 as M iTdO |TfO( n (4 (4 ss <4 | P V 'O |4 Dw 8 f4 M ftCL. w 6 o (4 v6 KX 0 fs| KK 41 ^ n K X w O o o M V0 o p 6* a e.a * >* 5 2 B 8 63 1 aV 3 2 S foi 3 4 U* eM mI - O o - n en Hp4I U"4*i n NEV 010076 WATER PCB-00051212 .. .. .. - { f). . t Si P. Wheeler - St. Louis October 21, 1968 Polychlorinated Biphenyls In the Environment . .* * . W. R. Richard . WRICK R. E. Kelly, M. D-/.W. RKELL- 7^.., * t^u* & C. Payton - CPAYT H. Bergen - UBERO W. K. Johnson - WJOHN a Attached is a Xerox copy of a technical paper which Scott Tucker and I picked up in Washington recently. This was provided ub by Donald A. Spencer of the National Agricultural Chemicals Association. Mr. Spencer requested that the paper be held "confidential" until such time as it may be published. Spencer indicated that if this paper were distributed one of his principal "sources" would refuse to give him prepublica tion information in the future. . Rlsebrough1s presentation (the attached) was made at a meeting of 20 to 30 toxicologists held at the University of Rochester in June. The meeting was billed as "The First Annual Conference on Toxicologyf"and was underwritten presumably by the AEC which has had contracts at Rochester for many years. Attendance was by invitation only. The meeting dealt "exclusively" with pesticides with about . one-third of the papers relating to mercury. As far as Spencer knows the papers, including the attached, will undoubtedly be printed as proceedings ,of the conference although I suspect individual authors were given permission to publish elsewhere. * * * In a few words, Rlsebrough has found PCBs along with chlorinated pesticides in a number of species of fish and birds along the California coast as well as in waters off Baja. California and Central America. He further reports FOB in fish from the Channel Islands and Puget Sound. No PCB was detected in the liver of tuna taken in the Galapagos Archipelago. * Scott Tucker is going to scrutinize the analytical aspects and particularly the validity of some of the assumptions made by the author. CS . Attachment , ' \ . . * * ' .' \. Elmer P. Wheeler. .. 0 5 DEPOSITION i EXHIBIT 1 36 1______ Nev 022116 WATER PCB-00051213 % MIMUTS OF MEETING OF THE CORPORATE DEVELOPMENT COMMITTEE November 17, 1969 Present; .. . ' Messrs. * E. J. Bock, Chairman H . H. Bible J . R. c k J. L. Gi1 1 is E . J . Putzell C. H. Sommer J. N. Ehlers, Secretary ORGANIC DIVISION, LAW AND MEDICAL DEPARTMENTS -- REPORT ON POLY CHLORINATED BIPHENYLS Present: Messrs. C. J. Smith, J. Mason, T. K. Smith, H. S. Bergen, J. E. SprInggate, R. E . Kelly, E. P. Wheeler, Rodney Harris, Jr., D. W. Miller, W. C. Robinson Monsanto 1s worldwide Aroctor business_amounts to 104 M lbs./yr., 70M used In functional fluids and 3^ M in plasticizers. This represents $22 H in sales. Products range from monochlorobiphenyl WATER_PCB-00051214 78. to decach1orobipheny 1 , terpheny 1 s , and chlorinated terpheny1s. Production locations are a t Annis ton, A1abama, Sauget, Illinois Newport, U.K. and Yokkaich1 , Japan. . ' Environmental Aspects - E. P. Wheeler The 5 and 6 chlorinated biphenyls (Aroc1 or 12 5^ and 1 260) have been found a t 1imited 1 oca tions in water , in birds and some forms of aquatic life. Recent indications are that such biphenyls may affect reproduction of fowl life and may be toxic to shrimp. These products are not toxic from the acute standpoint to man or fish but there is some evidence of ecological buildup in certain water deposits, in fish and ultimately in bird life. - Aroc1ors 1248 and 1ower in number are believed to be biodegradable but this has not been conclusively es tab 11 shed as yet. p Plan of Action - H. S. Bergen and J. E. Springgate The availability of alternate products to satisfy customer requirements was reviewed. Main problems are that no replacement product is available for capacitors and replacement products for other uses pose a pollution problem. In plasticizer uses, evidence Is not available as to whether Aroc1 ors escape from end products, either through leeching or by dispersal in burning. . t. . .' The .recommended plan of action is to establish a tailored program for each business groups and each customer market situation to assure that the loss of PCB' s in the environment, 1f any, is minimal. NEV 1.76945 ** WATER PCB-00051215 73. I. Appoint a Project Manager - responsible for the overall management of the Aroc1 or pollution problem. He would be assisted by a Task Force from members of each business group plus Medical, Law, Engineering and Manufacturing. 2 ., Notify all Aroc1 or cu s tome rs of PCS problem. 3. Reduce and effectively contro1 PCS effluents from Monsanto plants. ' 4. Educate customers on need to reduce and effectively control PCB eff1uents at their plants. 5 Develop and implement new packaging systems for Aroc1 or 1 25V 1260. . 6. Introduce to market, replacement products for Aroc1 or 125V1260. 7. Continue and expand biodegradat i on test program with Aroc1 or series , particularly 12V, 1248 and 1254. 8. Continue toxicological test program. 9. Accelerate present analytical test program. 10. Determine feasibility and cos t of eliminating 5/6 Cl in Aroc1 ors 1242 and 1248. 2 11. Study incineration products. -1 12. Develop business plan to offer: - Monsanto Fluid Reclamation and Recovery with Enviro Chem. (Reclamation already under-way a t Findett.) Cost of this program is estimated at approximate 1y $400M SARE and $700M capital to change equipment. ' Conclusions: In light of the recent and developing ev i dence of a possible threat to certaIn species of bird and aquatic life, we should plan to discontinue the manufacture.of A r o c 1 o r s 1254 and 1260. The Division is instructed to develop a program to discontinue these products and report this to the Committee. The status of Aroc1 or 1242 should continue to be tested to determine whether it contributes to this problem. Other products which might be involved shou1d also be examined. (Excerpt to Messrs. H. L. Minckler, Rodney Harris, Jr., R. E. Kelly, T. K. Smith.) ' NEV 176946 WATER PCB-00051216 K PCS PRESENTATION TO CORPORATE DEVELOPMENT COMMITTEE I. INTRODUCTION: V'.* sire here today to acquaint you with the PCB (Aroclor) pollution problem and to secure your guidance and approval on a recommended plan of action. . Certain PCB's have recently been identified by various scientists along with DDT in fish, birds, and other wildlife. From the standpoint of reproduction, the PCB's are highly toxic to birds. In a few moments, Elmer Wheeler will describe the problem in detail. Our objective is to describe for you the basic problems, the is.sues Involved, review alternative courses of action, and suggest an action plan program for your approval. Tide is a serious matter, not only from the pollution viewpoint, but also because of the $? Mi worldwide customer business involved with resultant gi-ocs profits of $10 T5 and a not investment of approximately $9 13. In addition, there could be possible adverse legal and public relations problems leveled against Monsanto. Our Agenda will be as follov.T.: a - c* , CT4Q * Vs* SA*M**,^ A* 4^* NEV 176947 WATER PCB-00051217 -2- PCB AGENDA REVIEW I. INTRODUCTION * II. THE PROBLEM - DEVELOPMENTS INCRIMINATING PCB's - COMPLEXITY OF IDENTIFICATION - NATURE OF - SERIOUSNESS III. LAW DEPARTMENT VIEWPOINT AND RECOMMENDATIONS IV. EFFECT ON MONSANTO AND ALTERNATIVES V. FUNCTIONAL FLUID BUSINESS GROUP DISCUSSION - MARKETS, USES - SOURCES OF POLLUTION - CUSTOMER EFFECT VI. PLASTICIZER BUSINESS GROUP DISCUSSION - MARKETS, USES - SOURCES OF POLLUTION VII. RECOMMENDED ACTION PLAN * VIII. SUMMARY NEV 176948 C `{f- WATER PCB-00051218 3- By 'fay of introduction, the Organic Division and the Medical Department has been actively engaged for the last 18 months in developing facts and knowledge on this subject by personal visits to Universities and Industrial test laboratories, other worldwide producers, and other industrial collaborators, as well .is keeping abreast of all literature and news sources on the subject as well as funding a toxicological and analytical test program In excess of $100 M. We established an Ad Hoc Committee of both Business Groups and Medical which recently issued a report - much of which will be discussed today. We have learned a lot, but there is much yet to learn as you will hear. What arc TCP's? They arc polychlorinated biphenyls - better known to us as Aroclors. The next slide will quickly re familiarize you with our Arocldr business. ,wnj*7r.wi<n' NEV l?6949 it - ...... WATER PCB-00051219 MONSANTO WORLDWIDE AROCLOR BUSINESS pounds/year sales/year 104 H $22 M (70 M in Functional Fluids 34 M in Plasticizers) t ($16 M in Functional Fluids $ 6 M in Plasticizers) gross profit/ykar $10.0 TI ($7.5 M Functional Fluids . $2.5 M in Plasticizers) gross investment $13 M ($8.8 M net investment) ROI ' WORLDWIDE M/I MONSANTO PRODUCTION LOCATIONS: 10.5# 62# USA (2 plants, Anniston, Alabama Sauget, Illinois) UK (Newport) JAPAN (Yokkaiehl) ` OTHER PRODUCERS: Bayer, Prod elec, Caffaro, Flick, Kanegahuchi, and several Eastern European producers (all ex-USA) . A-y U K NEV 176950 WATER PCB-00051220 I 5- THE AROCLOR PRODUCT LINE CHEMICAL NAME TRADE NAME MONOCl ILOROBiriIENYL AROCLOR 1221 DICHLOROBIPHENYL AROCLOR 1232 TRICHLOROBI PHENYL AROCLOR 1242 TETRACHLOROBIPHENYL AROCLOR 12*48 PENTACHLOROBIPHENYL AROCLOR 1254 HEXACHLOROBIPIIENYL AROCLOR 1260 HEPTACHLOROBIP1IENYL AROCLOR 1262 OCTACHLOROBIPHENYL AROCLOR 1268 DECACHLOROBIPIIENYL AROCLOR 1270 TERPHENYLS SANTOWAX CHLORINATED TERPHENYL AROCLOR 5460 NATURE OP MATERIAL THIN LIQUID OILY LIQUID HEAVY MOLAS . THICK TAR V> SOLID V SOLID' N6V 176951 5 WATER PCB-00051221 Theie are theoretically 210 different isomers of chlorinated biphenyls. ' Monsanto entered the Aroclor market in 1930 by acquiring Swan Chemical Company. The first load of Aroclor went out of Anniston, Alabama to General Electric in 1931. Since then, the market has grown to one of Monsanto's most profitable franchises. This franchise is now being threatened ''"I L i " < ,L'1" A recently found pollution problems which Elmer Vflieeler will now discuss. '. II, The Problem (Wheeler) - see attached Appendix A III, Law Department Viewpoint and Hecommendations (French) Effect on Monsanto and Our Alternative Courses of Action As discussed, Aroclors 125^ and 1260 -- the 5 and 6 Cl ringed biphenyls are the ones most seriously involved in the pollution problem. Both Plasticisers and Fluids Groups are involved as shown: NEV l76952 WATER PCB-00051222 AROCLOR SALES (M POUNDS) AROCLOR 121^1 AROCLOR 1260 & ABOVE FLUIDS 1.45 3.7 5.15 PLASTICIZERS 5.4 ill 7.1 TOTAL 6.85 5.*+ 12.23 i N6V 1,S1 WATER PCB-00051223 We considered 4 alternative courses or action; (Slide) Alternative 1: Do nothing was considered unacceptable from a legal, moral ad customer , public relations & company policy viewpoint. This is also the quickest route to being forced out of business. Alternative 2: Go out of total Aroclor business was considered unacceptable from a Divisional viewpoint, but from a Corporate viewpoint may be necessary. Only-you-can-make-1hafc-de ci-s io n. All Aroclor products are not serious pollutants - many degrade; there is too much customer/market need and selfishly too much Monsanto profit to go out. To go out would require a write off of Aroclor net Investment of $7 M (10//share) or if biphenyl included $8.8 H (12^/share). In addition, Inventory disposition, continuing cost of utilitiv.-s, and back-up capital and serious manpower & resources reallocation at Anniston. Alternative 3: Go out of Aroclor 1254 and 1260. This was seriously considered and may eventually occur by our actions and customer actions, nevertheless, we foci that segments of this business are defensible or arc so "confined" in use that specific plans of action are called for this portion. Our reasons for eliminating this alternative will become clearer as we outline our action plans. WATER_PCB-00051224 ALTERNATIVE COURSES OP ACTION 1. DO NOTHING - JUST REACT TO LEGISLATION AND EMOTION. 2. GO OUT OP TOTAL AROCLOR BUSINESS. 3. GO OUT OP AROCLOR 1254 AND 1260 PRODUCTION 4. DEVELOP SPECIFIC ACTION PLANS "TAILORED" TO EACH BUSINESS GROUP AND EACH CUSTOMER/MARKET SITUATION TO "CLEAN UP" THE MESS. I NEV H6955 S WATER PCB-00051225 Alternative 4: Develop specific action plans .tailored to each Business Group and each customer/market situation, - was the alternative selected at this point of time and based on our knowledge from a Divisional viewpoint as making Monsanto act in the most positive, responsible way to society and our customers, as well as our interests. ' However, because of the magnitude and seriousness of this pdf.}'' problem and its total implications for Corporate Monsanto, (/f .. .. t- . i' <'// - l '/ A; " ^he fina^ decision on this matter must be made by-the CDC. Functional Fluids Business Group Discussion: Aroclors are'used widely in 3 of our ^ market areas in the Fluids Group: ' NEV 17^956 WATER PCB-00051226 FLUIDS USE OF AROCLCRS BY MARKET AREA AROCLOR PRODUCT DOMESTIC MARKET AREA INDUSTRIAL HEAT TRAi\'SFEH ELECTRICAL TOTAL 1242 1248 121>4 . 1260 & Above 4.1 1.2 0.6 5.9 1.1 36 41.2 1.0 - 2.2 0.1 0.8 0.9 - 3.5 4.1 2.2 . 40.3 40.4 NEV i7C>9&7 s WATER PCB-00051227 SOURCES OP FLUIDS POLLUTION APPLICATION INDUSTRIAL FLUIDS DIELECTRICS HEAT TRANSFER PRODUCING PLANTS ' INTENSITY OF POLLUTION CREATEST (DIRECT) (INDIRECT CONTAINED) (INDIRECT CONTAINED) LEAST (DIRECT) NEV 17695a s WATER PCB-00051228 -1^- ' FLUIDS CUSTOMER ALTERNATIVES AREA OF APPLICATION Industrial Fluids Transformer Capacitors Heat Transfer PRODUCT OF CHOICE CUSTOMER OPTIONS Pydraul 312/F-9/ Customer could get along A-200/Phosphate Esters/ without us, but Pydraul Water Glycol 312 favored. H?0 Glycol has some pollution problem Phosphate ester route ok at present. Air/Oil/Aroclor/Gas Could drop Aroclor at sacrifice of safety, cost or size of equipment or noise level. Aroclors No immediate replacement available. Longer term oil at expense of size and cost of efficiency and redesign of equipment. Therminol Oil/Dow therm/T66 . T55 T?7 TQ8 No option for FR liquid market. Other system possibility. Liquid systems favored. T66 and T55 Increasing rapidly in use. Oil also a pollution problem. nev ITO'59 WATER PCB-00051229 Customer Choices &; Alternatives & Penalties: Summarizing, some of our customers have no immediate alternative, some could change only at sacrifices of safety, or cost or various technical factors. Only in the Industrial field could the customer make an immediate conversion. . PCB Threat to Functional Fluids Business and Profit: NEV 176960 WATER PCB-00051230 FLUIDS BUSINESS THREATENED (1970 BUDGET) PROBLEM Confined to A-1254/ 1260 only. Spreads to A-1242 and 12*18 First to: a) Industrial Fluids Then to: b) Dielectric Fluids Then to: c) Beat Transfer SALES $ 3.0 M GROSS PROFIT $1.38 M " $ 4.0 M $1.6 M $ 8.0 M $3.8 M $ 1.0 M $16.0 M $ .6 R $7.36 m 7W 'y. 7/ NEV 176961 WATER PCB-00051231 PLASTICIZERS (i:or:cjvuide) i.A>/ SJ'J/s.Sj ECLLAMS POUaDS *\ o L \y o> V*. (D ca V* A X ALL /.RCOLORS c? O 0 ,*i 3'voO K $ 2.5 K AROCLCR 125A/1260 Ti P $1.7 K ( ) 9.5 H V 20/i; $0.8 X (32#) NEV 176962 WATER PCB-00051232 -16- co: :TS: DlSTuTCTIOSS FROM F. F. 1. I .urge number of direct U.S. customers - 570 2. Customers are small: 23 direct customers - kV/ A-125Vl2oO sales, 3 50/* domestic A-1234/1260 sales through distributors - difficult to police. NEV 176963 WATER PCB-00051233 n '.A'AKV'.TS ' C vrbonloso Carbon Paper Hot Kelt Adhesives Sv;fi.!::dn>j fool Paints Protective Coatings 11.u lei or. Adhesives Soelante Modi :\i citron Kir. cel la .ecus j 959 SALES 8.8 `M lb. . 5.7 W lb. 1.7 K lb. 5.3 M lb. l.p K lb. 3.0 W lb. 2.0 K lb. 5.0 M lb. MAJOR AROCLCR 'JS2D Aroclor 1242 Aroclor 5450 Aroclor 12-V' Aroclor 5'vSc) Aroclor IZy.V' Aroclor 5J.b:) Aroclor 125-;) / Aroclor 1260 Aroclor 1251) Aroclor J-2-o 2/ Aroclor 10..nmr,./A/ . / Aroclor Aroclor i?- if./ Aroclor 'I- ) J ^ 1, :> tv; stajor eoeto.\.er (857S of Aroclor i2*'-2 sola}. of do:no..;ic- Aroclor-s sole! .;hrou_:n ..trl.-v.o:'-:. NEV 176964 WATER PCB-00051234 POSSIBLE CCXTAXUATION SOURCES (PLASTICIZERS) MARKET APPLICATION SOURCE Costings Marine Paints) Leaching Later tame ) , linings ) ' Coatings Sv;ir;i^lns Pool Leaching- Paints . Cnrbonlo.sc - Vaporization Carbon Paper . V/zix Mo dil'i cation - Vaporization Emulsion Adhesives Contact v.'ith product via packaging. In cineration. Lot Molt Adhesive- Contract with product via packaging. In cineration. ' Soslani s Automotive Long-term. lc-aching (41 ll') 'i lv* * C \*0.1 cu.?.x, r.orw'-^.ncs IS h-l25L'r /1260 USED? Yes Yes ,.;o Yes Yes No a.W tf.a> UU^ Arcelor plasticizers are cosv.bin.n. ir. o plastics *uC; <^OC4 vi (s i/.C final product - therefore, Par - os .obi ' .v. . lOido r.vch as wastes fror. our manufacturing plan to ..no iT.ci leasing of drums coitmon to both grot '..I' VJC ; or protective coatings are not considered Jo roc processing or NEV 176965 WATER PCB-00051235 II PLASTICIZER EUSIR/.SS T!-IRISATE^KD PRO v*>y* 1. Confined to A-lRl>-:/i260 typo only. SOI' to ail chlon > .ted bl phony. *..*ou S,^.. uu'ul.1 to a n .W. V**,*/..- >-/ * id aTJ. ch.V) .tod"' b W<a ^ a A S. a i j SALES R"T.:IKRL--:$4.3 :`>2.0 0.0 a.P. RETAINED (LOST) $1.7 T'l (-$0.8 h) $0.6 m (-$1.9 E) 0.0 (~$2.p h) s:,: on prospects S#v .... .<5 r 4 : . (/J. 8.'. sen >olor- 12o2/*i463 thich are very ooo to A.-IL'34/.lSoO and oho a o have boon included va A-liVl260. NEV 176966 WATER PCB-00051236 RECOMMENDED ACTION PLAN THE JOINT ACTION PLAN DEVELOPED BY THE FUNCTIONAL FLUIDS AND PLASTICIZER BUSINESS CROUPS, AND THE MEDICAL AND LAW DEPARTMENTS IS AS FOLLOWS: . 1. Appoint a Project Manager - responsible for the overall management of the Aroclor pollution problem. He would be assisted by a Task Force from members of each Business Group plus Medical, Law, Engineering and Manufacturing. 2. Notify all Aroclor customers of PCB problem and relabel containers - within 60 days, 3. Clean up Monsanto plants* effluents within 12 months. 4. Develop and implement new packaging systems for Aroclor 1254/1260 - within 6 months. 5. Educate customers on need for clean-up at their plants - within 4 months. 6. Introduct to market, replacement products for 'Aroclor 1254/1260 - beginning l/l/'fO (Fluids), 4/1/70 (Plasticizers). NEV 176967 WATER PCB-00051237 RECOMMENDED ACTION PLAN Continue and expand biodegratation test program with Aroclor series, particularly 1242, 1248 and 1254. Continue toxicological test program. Accelerate present analytical test program. Determine feasibility and cost of eliminating 5/6 Cl2 in Aroclors 1242 and 1248. (3/70) Study incineration products. (3/70) Develop business plan to offer: Monsanto Fluid Reclamation and Recovery with Enviro Chem (4/70). (Reclamation already underway at Findett.) I NEV 176968 WATER PCB-00051238 WHAT rXCLP WE EXPECT FROM THIS PROGRAM? Through. this action program* Monsanto would expect to: P.^-tain or convert a good portion of our business and profits: PHVBLJ5MS ' a. Confined to A-125V 1260. b, Spreads to A-12^8 and 22*12. CONVERT on RETAIN $20.3 M $10 H $M SALES OUT OF PRESENT $22 1 $22 M ODDS OF SUCCESS 70% 60# 2, n further valuable knowledge and time to: a. Learn more facts. . b. Protect our position. c. Make further decisions regarding our program. d. Contribute to overall pollution knowledge. 3, Clean-up the major contributing PCS pollution factors. 4, Minimize customer complaints and hardships. NEV 176969 WATER PCB-00051239 / The Program Would: 1. Cost some money. Esfc. SAKE - $*100-500 M Est. Capital - $700 M $1.1 I - 1.2 1 ' 2. Expose us to continued adverse publicity and possible law suits. ,, < 3. Cause some customer discontent - but much less than an abrupt termination of production. NEV 176970 WATER PCB-00051240 SUMMARY In summary, the PCB pollution problem is a very serious one. It Is a worldwide ecological problem. At present the most serious offenders are the 5 and 6 chlorine containing products (Aroclors 1254 and 1260). There are some indications other members are biodegradable to varying degrees. Currently, much l scientific testing is underway and more information will be forthcoming. Monsanto must act in a positive cooperative fashion. A plan of action has been discussed which we feel indicates responsible action. Our stakes are large and because of the many possible effects on the Corporation - your guidance and approval of the suggested action program is requested. Thank you for your consideration. May we answer any questions? NEV 176971 WATER PCB-00051241 fe ^*. GENTLEMEN; . . MY PARTICIPATION IN THIS PRESENTATION WILL BE A BRIEF REVIEW OF THE DEVELOPMENTS WHICH INCRIMINATE THE POLY CHLORINATED BIPHENYLS INCLUDING OUR AROCLORS AS NEARLY tffftfffitDE iWlRONMENTAl, QONTAMINA STATES; DEPLETION IN POPULATION OF THIS SPECIES IN CALIFORNIA; AND THE REPORTED EFFECT ON THE BROWN PELICAN IN CALIFORNIA. 3) PCB'$ ARE PARTICULARLY TOXIC TO SHRIMP. AT PENSACOLA, THERE WAS A LOSS OF 1 TO 3 GALLONS PER DAY OF AROCLOR 1254 INTO THE ESCAMBIA RIVER FROM OUR NYLON PLANT. THE RESULTANT CONCENTRATIONS OF PCB ONE-OUARTER MILE BELOW THE PLANT WERE ABOVE THE LEVELS NEEDED TO KILL JUVENILE SHRIMP IN LABORATORY TESTS. 4) THERE ARE STILL MANY UNKNOWNS BUT SPECULATION AS TO THE ROLE OF PCB'S IS RAMPANT. ' ALTHOUGH SOME, OF THE REPORTS OF ANALYTICAL IDENTIFICATION Ai*7 ARE* NOT -CERTAIN. THE MEDICAL DEPARTMENT--AFTER 18 MONTHS OF INVESTIGATION IN CONJUNCTION WITH THE ORGANIC DIVISION--IS CERTAIN THAT THE PCB'S CAN BE RESPONSIBLE FOR ECOLOGICAL DAMAGE. THERE IS NO SCIENTIFIC CONSENSUS AS TO THE DEGREE OF PCB INVOLVEMENT BUT THESE COMPOUNDS CANNOT ESCAPE A SIGNIFICANT SHARE OF THE BLAME FOR DAMAGE. NEV 176972 WATER PCB-00051242 55)) SPECULATION IS LEADING TO CONCERN WHICH MAY GROW TO ALARM. '. the MEDICAL DEPARTMENT BELIEVES THAT THE MYRIAD OF INVESTIGATORS PRESENTLY WORKING ON PCB'S IN GOVERNMENT AND UNIVERSITY LABORATORIES IS CERTAIN TO PROMOTE A MORE PROMINENT ROLE FOR PCB DAMAGE, LEADING AT BEST TO EXTREMELY DAMAGING PUBLICITY AND, AT WORST, LEADING TO COMPLETE BANNING OF THESE PRODUCTS. NEV 176973 WATER_PCB-00051243 CERTAINLY ALL OF YOU ARE AWARE Of THE PRESENT CONCERN ABOUT THE RESIDUES OF DDT, ITS METABOLITES AND OTHER CHLORINATED HYDROCARBON PESTICIDES THROUGHOUT THE WORLD. SINCE WORLD WAR II ANO IN THE LAST DECADE IN PARTICULAR, THERE HAS BEEN A SAMPLING NETWORK WHICH HAS IDENTIFIED DDT AND ITS METABOLITES IN PRACTICALLY EVERY LIVING ORGANISM 'AND'IN THE AIR, WATER AND SOIL ACROSS THE FACE OF THE GLOBE. IT WOULD NOT BE UNEXPECTED TO FIND THAT EACH OF US IN THIS ROOM HAS 5 TO TO ppm OF DDT IN OUR FATTY TISSUES. 0 AS ANALYTICAL TECHNIQUES HAVE IMPROVED AND INCLUDED VERY SENSITIVE GAS CHROMATOGRAPHY METHODS, INTERFERING SUBSTANCES HAVE APPEARED WHICH RAISE QUESTIONS AS TO THE VALIDITY OF PRESENT AND EARLIER DETERMINATIONS OF DDT MATERIALS. THIS DIAGRAM INDICATES THE GAS CHROMATOGRAMS OF SEVERAL OF OUR AROCLORS. AT THE BOTTOM THE PEAKS FOR VARIOUS HYDROCARBON PESTICIDES ARE SHOWN. IT IS OBVIOUS THAT SOME OF THE PREDOMINANT PEAKS IN THE AROCLORS FALL IN THE SAME POSITION IN TERMS OF RETENTION TIME AS DOT . ' N6V 176974 WATER_PCB-00051244 AND ITS METABOLITES. PLEASE NOTICE THAT THIS IS PARTICULARLY TRUE FOR AROCLORS 1254 AND 1260 AND IT IS THESE TWO PARTICULAR POLYCHLORINATED BIPHENYLS, WHETHER MANUFACTURED BY MONSANTO OR OUR COMPETITORS, THAT ARE THE, PRODUCTS WHICH ARE MOST CONSISTENTLY IDENTIFIED ( PENTA M--0TA~ CHLORO). LET ME EMPHASIZE THIS POINT BECAUSE IT HAS A PARTICULAR BEARING ON THE FUTURE MANUFACTURE, SALES AND USE OF THE WHOLE PRODUCT LINE. . WHERE HAVE THE PCB'S BEEN FOUND? THIS NEXT TRANSPARENCY INDICATES LOCATIONS WHERE THESE MATERIALS HAVE BEEN REPORTED. THE AMOUNTS FOUND VARY FROM PARTS PER TRILLION IN SOME WATER SAMPLES TO HUNDREDS OF PARTS PER MILLION IN FISH AND SOME FISH-EATING BIRDS. LET ME DIGRESS A MOMENT TO EQUATE THESE UNITS OF PPM, PPB AND PPT TO SOMETHING THAT WE ALL RECOGNIZE (SHOW TRANSPARENCY ON COMPARISON OF PPM TO FIFTHS). . RETURNING TO THE REPORTED FINDINGS OF THE PCB'S, THE VALUES THAT HAVE BEEN REPORTED IN SWEDEN VARY FROM 10 PPB IN FISH, BIRDS AND-EGGS TO 20,000 ppm IN ONE OR TWO SINGLE SPECIMENS. IN THE LATTER CASE, THESE HAVE BEEN DEAD BIRDS AND THERE IS SOME QUESTION AS TO THE VALIDITY OF THE RESULTS. IN REGARD TO CHILDRENS HAIR, DR. JENSEN HAS POINTED OUT THAT HIS FIVE MONTH OLD CHILD HAD MORE PCB'S IN THE HAIR THAN HIS THREE AND SIX YEAR OLD CHILDREN AND HE POSTULATED THAT THIS WAS DUE TO THE PCB BEING IN MOTHER'S MILK. THE SAME LEVELSOF PCB'S HAVE BEEN FOUND IN FISH, BIRDS, AND EGGS IN NEV 176975 WATER_PCB-00051245 -3- GREAT BRITAIN AND THE NETHERLANDS. IN THE UNITED STATES AS WE HAVE INDICATED, THE PCB'S HAVE BEEN FOUND IN IN-LAND WATERS. THIS IS QUITE DIFFERENT UP TO THIS POINT AS REGARDS THEIR DISTRIBUTION IN GREAT BRITAIN, IN THE NETHERLANDS AND IN THE SCANDANAVIAN COUNTRIES. l/pERHAPS I SHOULD REMIND YOU THAT MONSANTO IS THE SOLE PRODUCER AND SUPPLIER OF POLYCHLORINATED BIPHENYLS IN THE.UNITED STATES AND GREAT BRITAIN. THIS IS IMPORTANT SINCE ANY PUBLIC OR GOVERNMENTAL AGENCY ACTIVITY WHICH MAY LEAD TO THE RESTRICTION OF USE OF POLYCHLORINATED BIPHENYLS MAKES MONSANTO PARTICULARLY VULNERABLE FROM A PUBLIC RELATIONS STANDPOINT IN THE UNITED STATES, GREAT BRITAIN AND PROBABLY CANADA. IN TERMS OF TOXIC OR HARMFUL EFFECTS FROM THE PRESENCE OF PCB'S, WE CAN MAKES THESE STATEMENTS SUPPORTED BY A GROWING AMOUNT OF TOXICOLOGICAL RESEARCH DATA: 1. THE AROCLOR'S ARE NOT HIGHLY TOXIC FROM AN ACUTE STANDPOINT TO MAN, ANIMALS, BIRDS OR FISH. FOR ' EXAMPLE. THEY ARE NOT NEARLY AS TOXIC AS DDT AND CERTAINLY MUCH' LESS TOXIC THAN DIELDRIN AND ALDRIN. .. 2. FROM A CHRONIC TOXICITY STANDPOINT, THE PCB'S MAY BE CONSIDERED "MODERATELY TOXIC" TO MAN, ANIMALS AND FISH. FROM THE STANDPOINT OF REPRODUCTION, THE PCB'S ARE HIGHLY TOXIC TO BIRDS. THIS CON CLUSION IS BASED ON ON-GOING RESEARCH AT OUR . CONSULTING LABORATORY IN CHICAGO WHERE WHITE LEGHORN CHICKENS--A RELATIVELY RESISTANT MEMBER OF THE BIRD SPECIES--ARE LAYING EGGS AFTER BEING ' NEV 17*976 WATER_PCB-00051246 -4- ' FED A DIET OF 10 PPM WHICH FAIL TO HATCH. AT TOO PPM THE EGGS HAVE GREATLY REDUCED EGG SHELL THICKNESS AS WELL. IN THE AQUATIC ENVIRONMENT, SHRIMP APPEAR TO BE PARTICULARLY SENSITIVE TO THE PCB'S. IN A TEST CONDUCTED AT THE BUREAU OF COMMERCIAL FISHERIES LABORATORY, GULFSTREAM, FLORIDA, 5 PPB CAUSED THE DEATH OF 18 OUT OF 25 JUVENILE SHRIMP IN 18 DAYS. ALTHOUGH AT THIS POINT THE PCB'S ARE NOT BEING TOUTED AS SERIOUS TOXICANTS, THERE HAVE BEEN COMMENTS IN EACH OF THE PUBLICATIONS WHICH HAVE APPEARED WHICH HAVE IMPLIED-IF NOT STATED DIRECTLY--THAT THESE MATERIALS ARE "HIGHLY TOXIC". THE FUTURE OF THESE MATERIALS IS THREATENED MORE BY THE POTENTIAL EFFECT ON SOME FORMS OF WILDLIFE RATHER THAN POTENTIAL TOXIC EFFECTS AS WE USUALLY THINK OF THEM IN RELATION TO HUMAN OR ANIMAL FOODS. IN THE ENVIRONMENT WE ARE FACED WITH THIS CYCLE--FISH IN WATER CONTAINING PPB OF PCD CONCENTRATE THE MATERIAL TO PPM. THE SWEDES SAY THAT LARGER FISH EATING SUCH SMALLER ONES SHOW A (10 FOLD INCREASE IN THE AMOUNT OF PCB IN THEIR TISSUES. BIRDS THEN EATING THESE FISH SHOW 100 FOLD CONCENTRATION OF PCB FROM THAT IN THE FISH WHICH THEY HAVE EATEN. IT IS POSTULATED AS IN THE CASE OF DDT THAT THIS CONCENTRATION LEADS TO EGGS WITH LITTLE OR NOT SHELL THICKNESS AND WITH DECREASED OR NO REPRODUCTION. NEV 170^77 WATER_PCB-00051247 -5- MOW 00 THE PCB'S GET INTO THE ENVIRONMENT? OUR EFFORTS TO DATE HAVE NOT SEEN COMPLETELY SUCCESSFUL IN PIN-POINTING SOURCES OF THE PCB'S. AS MR. BERGEN AND MR. SPRINGATE WILl-DISCUSS SHORTLY, HE 00 HAVE SOME IDEAS CONCERNING SPECIFIC PRODUCT USES. WE CAN, HOWEVER, MENTION THREE INSTANCES WHICH WILL GIVE SOME IMPRESSION AS TO SOURCES SUCH AS OUR MANUFACTURING PLANTS, A MONSANTO "CUSTOMER"PLANT, AND EARLY RESULTS OF WIDE-SPREAD SAMPLING IN LAKE MICHIGAN (SHOW TRANS PARENCY OF SEVERN RIVER, PENSACOLA AND LAKE MICHIGAN). THIS IS AN INDICATION OF THE PCB CONCENTRATION IN MUD NEAR THE OUTFALL OF OUR NEWPORT PLANT. YOU WILL NOTE THE SCALE IN MILES AT THE BOTTOM AND THE DISTRIBUTION OF PCB ALONG THE ESTUARY OF THE SEVERN RIVER. SIMILAR FINDINGS COULD BE SHOWN FOR THE STREAMS BELOW OUR ANNISTON AND KRUMMRICH PLANTS. AN INDICATION OF "CUSTOMER" USAGE AS A SOURCE IS INDICATED IN THIS SLIDE. THIS IS A MONSANTO CUSTOMER PLANT WHERE THE PENSACOLA INSTALLATION WAS USING FIRE RESISTANT AIR COMPRESSOR LUBRICANT CONTAINING AROCLOR 1254. IT WAS REPORTED THAT ONE-FOURTH'MILE BELOW OUR PLANT OUTFALL, 40 PPB OF PCB WAS PRESENT. AT THE BRIDGE AT HIGHWAY 90, 0.5 PPB WAS REPORTED. THE STATE AND UNIVERSITY IN DOING FURTHER SAMPLING REACHED IN BEHIND THE SKIMMERS ON THE OUTFALL OF OUR PLANT AND FOUND PPB. N6V 176978 WATER_PCB-00051248 .. . -6- AS A FURTHER EXAMPLE OF THE POSSIBLE SOURCES FROM OUR CUSTOMER PLANTS, THIS 1 TRANSPARENCY SHOWS EARLY REPORTS OF SAMPLES FROM LAKE MICHIGAN. WATER SAMPLES HAVE SHOWN PARTS PER TRILLION TO PARTS PER BILLION OF THE HIGHER CHLORINATED BIPHENYLS. WHEN WE BROUGHT THIS BACK TO OUR MARKETING GROUPS, THEY QUICKLY POINTED OUT THAT ONE COULD ALMOST PIN-POINT OUR CUSTOMER USAGE ALONG THE SHORES OF LAKE MICHIGAN. THESE THREE INSTANCES REFLECT WHAT MIGHT BE TERMED DIRECT CONTAMINATION. AS YOU WILL HEAR, THE POSSIBLE SOURCES OF INDIRECT CONTAMINATION MIGHT BE RELATED TO EVERY SINGLE USE OF OUR PRODUCTS WHETHER THE USES BE IN ELECTRICAL APPLICATIONS, OTHER INDUSTRIAL FLUIDS, OR PLASTICIZER USAGE . THE SCIENTISTS WHO HAVE PUBLISHED THEIR FINDING OF THE PCB'S IN NATURE HAVE IN EVERY INSTANCE MENTIONED THE POSSIBLE SOURCES AS THE LIOUID MATERIALS AS INDUSTRIAL ' POLLUTANTS AND THE PLASTICIZER USES WHERE IN THE MANUFACTURE OF A PLASTIC MATERIAL SOME VAPORS ARE LOST TO THE ATMOSPHERE AND ULTIMATELY END UP IN THE OCEAN AS CHEMICAL FALL-OUT. o-nv HAVE THE HONOR IF IT BE SUCH OF HVINj\JHIS 0l'0TE0 IN THIS NEW BOOK ON CHEMICAL FALL-OUT. ' *hW HAVE POSTULATED ALSO THAT SINCE THE PCB'S ARE VIRTUALLY INDESTRUCTIBLE, EVERY POUND EVER MANUFACTURED ULTIMATELY HAS ESCAPED INTO THE ENVIRONMENT AND REMAINS THERE. AS FAR AS FUTURE ACTION IS CONCERNED, THE MEDICAL DEPARTMENT PROPOSES TO CONTINUE A PROGRAM, AND I MIGHT ADD--AN EXPANDED NEV 176979 WATER_PCB-00051249 -7PROGRAM--WHICH WE HOPE WILL PERMIT THE CONTINUED USE OF AROCLORS 1254 AND 1260 IN THOSE APPLICATIONS WHERE ESCAPE` INTO THE ENVIRONMENT CAN BE POLICED AND PREVENTED. SECONDLY, WE HOPE TO DEVELOP DATA THAT WILL SHOW THAT THE LOWER CHLORINATED BIPHENYLS, THAT IS--AROCLOR 1242 AND THOSE LOWER IN CHLORINATION, ARE DEGRADED IN THE ENVIRONMENT AND THUS DO NOT PRESENT A THREAT TO WILDLIFE. THERE IS SOME INDICATION FROM WORK UNDERWAY IN RUABON THAT AROCLOR 1242 WILL INDEED DEGRADE BIOLOGICALLY. THERE IS A PUBLISHED REPORT FROM THE UNIVERSITY OF UTRECHT WHERE 1242 FED TO QUAIL SHOWED VIRTUALLY COMPLETE DEGRADATION. AS I HAVE MENTIONED EARLIER, EXCEPT FOR ONE OR TWO INSTANCES AROCLOR 1242 HAS NOT BEEN IDENTIFIED ALONG WITH THE PESTICIDE RESIDUES. THIS IN ITSELF SUGGESTS THAT THIS MATERIAL IS DEGRADED. WE WOULD HOPE THEN THAT OUR EFFORTS WILL PROTECT THE CONTINUED SALE AND USE OF AROCLORS 1242, WHICH AS MR. BERGEN AND MR. SPRINGATE WILL INDICATE', MAKES UP A MAJOR PORTION OF OUR AROCLOR BUSINESS. WE WOULD BE LESS THAN HONEST HOWEVER, IF WE DID NOT POINT OUT THAT THE SCIENTIFIC DATA TO BE DEVELOPED FROM OUR OWN RESEARCH AS WELL AS BY ANY NUMBER OF THE 50 GOVERNMENTAL OR UNIVERSITY LABORATORIES THAT HAVE REQUESTED SAMPLES OF AROCLORS MAY NOT BE FAVORABLE REGARDING AROCLOR l. IN SUMMARY, THE MEDICAL DEPARTMENT FEELS THAT LONG-RANGE/. THERE MAY BE LESS THAN A SOX CHANCE OF SUCCESS IN PROTECTING NEV 176960 WATER_PCB-00051250 -8- THE MARKETS FOR THE POLYCHLORINATED BIPHENYLS. WE FEEL THE ODDS DEPEND ON AT LEAST FIVE FACTORS BEYOND OUR CONTROL: 1. WE MAY FIND THAT THE PREVENTION OF ESCAPE OF THESE MATERIALS TO THE ENVIRONMENT IS IMPOSSIBLE-- EXCEPT IN VERY LIMITEO APPLICATIONS. 2. ALTHOUGH, AS I HAVE INDICATED EARLIER, THERE IS SOME EVIDENCE THAT THE LOWER CHLORINATED MATERIALS SUCH AS AROCLOR 1242 ARE BIODEGRADABLE, FURTHER RESERACH SPONSORED BY MONSANTO OR OTHERS, MAY PROVE THAT THIS IS NOT THE CASE. 3. WE CANNOT CONTROL THE EFFORTS OF THE CHLORINATED PESTICIDE MANUFACTURES WHO--IN DEFENSE OF THEIR PRODUCTS, DDT AND THE OTHERS--HAVE BEGUN TO EMPHASIZE IN GOVERNMENT HEARINGS AND SCIENTIFIC SEMINARS 31HAT THE PAST AND CURRENT RESIDUE ANALYSIS MAY BE UNDULY ALARMING BECAUSE OF THE PCB INTERFERENCE. 4. IT WILL BE DIFFI CULT--1F NOT IMPOSSIBLE--TO COUNTERACT THE EFFORTS OF OUR COMPETITORS IN THE FUNCTIONAL FLUID APPLICATIONS WHO HAVE BEGUN TO BROADCAST THE POTENTIAL PCB PROBLEM--NOT ONLY TO OUR CUSTOMERS BUT TO REGULATORY AGENCIES SUCH AS THE MICHIGAN DEPT. OF NATURAL RESOURCES, AND 5. WE MAY FIND IT IMPOSSIBLE TO COUNTERACT THE EFFORTS OF THOSE SCIENTISTS AND PSEUDO-SCIENTISTS NOW INVOLVED IN THE U. S. AND EUROPEAN WILDLIFE CONSERVATION EFFORT WHO--TO PUT IT MILDLY--DO NOT ALWAYS REACT RESPONSIBY. ' \' NEV 176981 WATER_PCB-00051251 6 HAVE AROC AS YOU CAN IMAGINE, WE IN THE MEDICAL DEPARTMENT HAVE BEEN CONCERNED DURING THESE MANY MONTHS ABOUT THE .POSSIBILITY OF LEGAL AND FINANCIAL LIABILITY WHICH. MAY FACE MONSANTO IN THIS SITUATION. `IWBrf-RENCH IS NEXT ON THE PROGRAM TO DISCUSS THIS ASPECT Of THE PROBLEM. NEV 176982 WATER_PCB-00051252 i1s 1) THE 5 AND 6 CHLORINATED BIPHENYLS--OUR AROCLORS 1254 AND 1260--ARE PRESENT IN THE ENVIRONMENT, IN BIRDS, FISH, AND OTHER AOUATIC LIFE. , ' * 2) THESE, IN PART OR SOLELY, ARE AFFECTING REPRODUCTION OF SOME SPECIES OF BIRDS. 3) PCB'S ARE PARTICULARLY TOXIC TO SHRIMP. 4) THERE ARE STILL MANY UNKNOWNS BUT SPECULATION AS TO THE ROLE OF PCB'S IS RAMPANT. * 5) SPECULATION IS LEADING TO CONCERN WHICH MAY GROW TO ALARM. NEV 176983 WATER PCB-00051253 j i:.oa `jn,v.*u/.?.o(:'/.ao |] fii* AmlyiiB of *- `...... ctclot racldutf. Chron.A purified eagle extract* ChronB* - purified eagle extraot at above after nitration* Chroa. C.-polychlorinated biphenyl aolutlon a. Coluan 6 % Q? 1, EC-deteotor , f jf v 5 'i - -V-' ` it 6 is m . v. A / W./ __JL_ NEV 176984 WATER_PCB-00051254 1 PART PER MILLION --- 1 DROP IN 90 FIFTHS 1 PART PER BILLION --- 1 DROP IN 90^000 FIFTHS OR --- 1 OUNCE IN 1,000 TANK CARS NEV 176985 WATER PCB-00051255 NEV 176986 WATER PCB-00051256 ffa r u 'S *n WATER PCB-00051257 345 1 INDEX 2 3 THE WITNESS: ROBERT EMMET KELLY, M.D . VOLUME III 4 5 EXAMINATION: PAGE 6 By Mr. Kim (Continued) .............. 349 7 8 KELLY EXHIBITS: 9 Exhibit No. 38 350 "Report of Dr. Frederick B. Flinn 10 of Patch Tests Made on Material Received from Swann Research, Inc., 11 Dated May 25, 1954 12 Exhibit No. 39 .......................................... ............... 375 "Medical Research Project No. 13 MR-4 6, The Toxicity and Potential Dangers of Inerteen," Submitted by 14 W. F. von Oettingen, M.D., Ph.D. 15 Exhibit No. 4 0 .......................................................... 378 "The Toxicology of Inerteen and 16 Related Substances Including a Method of Analysis for Halogenated 17 Hydrocarbons in the Air," by A. J. Fleming, M.D. 18 Exhibit No. 41 .......................................................... 378 19 "The Effect of Inerteen and Several Related Substances Upon the White 20 Rat," W. T. Read, Jr., M.D. 21 Exhibit No . 42 ................ .............................. .. 4 33 Letter Dated February 14, 1950, 22 to Dr. Louis W. Spolyar from R. Emmet Kelly, M.D. 23 Exhibit No. 4 3 ....................... 438 24 State of Indiana, State Board of Health, Letter Dated February 28, 25 1950, to Dr. R. Emmet Kelly from L. W. Spolyar, M.D. Martin & Associates ( 409 ) 762-2222 WATER PCB-00051258 346 1 Index (Continued) 2 3 KELLY EXHIBITS: PAGE 4 Exhibit No. 4 4 ....................................................., 465 Memorandum Dated December 12, 1966, 5 to Mr. D. Wood from R. Emmet Kelly, M. D . 6 Exhibit No. 45 .................................................. 468 7 Memorandum Dated December 1, 1966, to G. R. Buchanan from D. Wood 8 Exhibit No. 4 6 ............................................. ............. 480 9 Monsanto Memorandum Dated January 12, 1967, to P. G. Benignus 10 et al, from D. V. N. Hardy 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 Martin & Associates ( 409 ) 762-2222 WATER PCB-00051259 493 1 INDEX 2 3 THE WITNESS: ROBERT EMMET KELLY, M. VOLUME IV 4 5 EXAMINATION: 6 ? By Mr. Kim (Continued) PAGE 496 8 KELLY EXHIBITS: 9 Exhibit No. 4 7 .......................................................... 497 Monsanto Memorandum Dated 10 January 26 , 19 6 7 , to G. R. Buchanan from D. Wood 11 Exhibit No. 4 8 .......................................................... 500 12 Memorandum Dated February 13, 1967, to R. Emmet Kelly, M.D., from Gene 13 Wilde 14 Exhibit No . 4 9 ............................ ................. .. 589 Monsanto Memorandum Dated June 12, 15 1956, to Dr. R. Emmet Kelly from Elmer P. Wheeler 16 Exhibit No. 50 .......................................................... 589 17 Monsanto Memorandum Dated June 12, 1956, to Dr. R. Emmet Kelly from 18 Elmer P. Wheeler 19 20 21 22 23 24 25 Martin & Associates ( 409 ) 762-2222 WATER PCB-00051260 / 8 19M Don or io Hama: a# ninr ov mwe *an m ow iubhiiil mwiB nai wrM miiM, m. fha *)Mt A thla iatoatlcatloa na to Aotoadaa vbttktar Mt tto wliu okloxiaatoi ilpk7l aa|ffito aataittod or -- lapriliM e^Mlaim! thorala Mfkt to tto aaaaatlTa agoa* pwdnola* tot daxxatltla Alek ted daralopA mbs im of tha voztaaa la too plot* ' larp Alto rabbito aaoA la asieiai tto patok testa to litolM tto Mtlom cf tto Tarleoa aMm&e&m aatelttod m tit Aim<> fko p>oaafttEra tis to akata tko salael i boom bAera tto pAeh mm appllod ttot tkara wmM It ao brokaa Ms to iatarfara Ato a* to aggravate tto taat f& Material tolag taated mm Mmg Ate atkpl laokol alt tor gattlag a aslvtiam ar a MjiaAoa far Iko pvpM @f AUvtiac tto asttrtd,# fko patok vaa laft <m tm mAom parida Aarlag tto toata -- mm for IIS ten* otbaro fa* <18 ten Ika patok was tkes ronovod ad' tto ozpoaad araa eatokA for toe mki to ba tor* that tha toat u aogatlia* fhla wm im to mil tea aknoa of aot <ti>ervtsg My laftoat ar dalsyai aot ion amh m le taatliM taka plaaa is aaklag patok test0a W@s mm mm irfesmtlom tto aakociala vtttk wm aocatito nn oppUM 1m a esaeaiSgestM faa ia &a?M6et toata to mm if a damatltla olgkt ask daTalop vte tkaaa tiromituaM* ladtpmimt toata mm mM Ate aaok sctwlal aad mm sii on lilfimt daya Aik frotely pimi aeXatloaa to to aora that M amr had oxipt is* Coatrollad toata vara mMa .aaak Mm# Atk tto alookol ad gniaa ad to dato^M wtottor tkoy Aght sot to tto asctlT agtat aMag tto stamt IoAobb* (Km balao ia Riaea rpostf toEisg doAffmtloa Him too v&Amm sisiesiaSs ty tew ItMvok foUwf kjr Sto MMMo fiaaisatim eM mill f Mak Aaolfia aalvtals iroalag IMt 9, wiM ktfora . iroler isigg Xt Ml GSgM) tost* w &-) . tw toiti Ato wantnA smtaiiel les eiss aegaMm M iatwiiaitl iaa ttpllfti ^ __. XWf pace lft$ by Bni* ,Aioa1 aai 4>rf atnaaa A atyroM Aak beilan __ _ irealar H ltt latoboek 176t pca ltt aaa aapatlA to all fMta tesleiias tto niuidlnM si, Islnltiiuli -^n\ EXHIBIT mo < A I JHMMxdi 2 0 5D WATER PCB-00051261 u \t ; / Mxmhn ipoold (Lot l&tmteek Vo. lit, mm t| ynpmA bp cf vq( diphenyl ad Mj( otyrae ad' atyroao M# toilwK (Llqgld itooicr. aalfio awitr ixoolor Special XftMMic Yo 198* pc* Sr- m ehaleal avo podtla test vllfe taok of Ik elht applltstlons* It Am pn poettlm apltoi Mm Ik fmiM4uil toot* Bo tjpi of domotitla mo ftlA* _ _ iIQ.l 1M (Lot . !. 3/M/M) toil* iMi, Let f| Ml eight testa pn o poalti* reaetia* *he lohrademal teat tu Mm positive* A* mitin mo aSMo Asmlm laii tot 8a sit g/i/i8h '` Imior ims0 lot 9 A elgfeS testa govs a positiie roaatla witk this scopoud# Istraderaal teat ms Mm paitiw X fool that tka Aemtltla produced %j tkla aatezlel vaa prevtoua" GssafSaMa iMel mee Mm ftooad, to b# perttite* fit aatorel teats it did Ml mko its ipimN fa M hours after tko gate! Mi tom naowi# .teeoloy tM9 (Lot la Iter gyoanat sale g/m/sili Jroelor 1S69* lot 8@ vonl itp Ml eight teeta war* negative* *he ia true of the too taata ante 11t the ooaooatwtei aaterlel* fhe iatrudeaal teat gave reeetiOB*' ' Imkr H89 CM letateek ITS* page IM4 ppinl bp Barrie* of S6*8J( diphenyl and d*8p etyzene oad etrraao Mil holler -- irfr oaotadl iroolar iSISo lot notebook ITS, pc 111* <17 vomit Ml eight tosta mre aespiflm 'a oaeostrmtei testa ueze Mot negative* a klnitiitl test gsto apatite smotioa* ' koite UH &t Sijl>salg Be* ITS* pig .- - ' IMI| Let l8teh#k ITS I ptt ML* mt great* Ml el^il teste men opllitt Be too toota isis vttk ooneaatratod material mre alee aogallvo* Be Ulnltad test gw a negative natlab iswlar list* Let 9# IMtMk * 19*, 8W IQ Cflw around la <! MUit .. ' iroelar S3S0 lot S Isteteek 5teo ItSf gego Ut GigSsti gsfi!i taste mcgatiWo tt testa rate vlth oonsaatratad odazlal mro 9lm a^tlw fko ialmdaaal taata *va a aacitlta matlea* 6BRN002056 I WATER PCB-00051262 MnlO #M00 bloaax JUOOi Tfela eoapeoad a peAti1** test la oil g Ifce eight tests is rtlafc it m applied* fha nastte vu different fxot that af tha tfcrea MrnAsm gitiag a paaitlva reastloa* mm vava aIM0 l)ii Ilia arterial gave am 2/i#irtlm area* Mimftfltti * . Bttewx Mi ISA tests Mth %Ma eoapomd) toth and dilate, vara upUtt* '& Salewa #10041 Ihlonax loots Ml tart* rttfc this arttrial toil sessnlnt*! and 4Umte, 83 mdioti-Wo gtrrene Bichloride (Notebook Ie lft. mm Hit . """ "iltfrittt 'BiohleriCdes aide ilttMi aaterlal mm pealtiae* Zt noticed tfcrt the rabbit poUM mm teas this ehealeal waa applied w la the dilrta {m fhla Am mm m Aaeratlie leaden* Aroalor la4fl mmiel (Batch i6 aplo 04 - --ifla lo/i/mh drooler IM8 Special Batch S>0-4* Isle UO/i/dOt Mi tain gave a Tarj aligkt raaatlaa rtth the akla bat oae anrt sagr that it la pAttfh ' drooler lum (lot 88. im&Q d/c/glli tamlm 1M0 Sat 8t* Brta /*a/ZL)t m Am tasta vara mmtiwt lb iaMmii ar concentrated taata vane node* itmIb isii (latch ba. iad y.if-e. Mi T/a/ao) drooler IMS* latch 8A IM T//* dll testa care negative* ite ltM. Hmw (IQteboolc po* Htjgigo gLli Ms? ethyl banseao* Ittilrt ttt, page SLt Iwsy teat sate Mm thla mrtenlal gate a paaitlie teat* tta lasiaa vaa at . oloerntlve jpa* . _# Chlorinated Stprano (iateltaakj>J,tt,_ggiJAj^LfiA^ .' Chlovftaetcft Stprane. Votabook Its, pa* If t/U/lto STary tart node vlth this eonpoond gave aa ahierrtlte leaden* GBRN002057 s WATER PCB-00051263 4 to* lllaa*a NKOkl T4 Bfidt WMIll, Gffl fOllOtat Oaa Sa vitk tto foot tM Mb f tba iMm Cltlac a positive wasttoa m af a tlaii aataro* Utopia vara eala to ii}i tha ttSsais to v^ara tens ebaarrefeloea meMm m ooaolada tbal tbo obIj fttftran ia that tba laal voaM to oopooed to tho bo% utoslal cat it *aa toll taoM tbat la nutlti abort Mb aa upeiaii is proa la mm ammso ' ' Oaa wwl tot foal that aajr itpiw lapml ablab asf to iooad to bo praoaat qs ea l^wity la tbo taa ef jew troabla* Z M ratbor tbal sag ef. tba aalolttal tit aat ahoa or pvt mstloaa tba Mx# It baa beta atom la msm _ lBveatlgatlOBa tbat ahlorlaa 414 asl predito a iozaatltla Am ' IKpliiflf aarbM alaatrodaa* Si tbaory aaa dnasil tlul ess mwmta ahlorlaa 9E3gsiia voro psofcoot tm tbo latta* Z waM aocpat till je atody f&m vaPUatloa ajatoK la plaooa abort ftaoo art pvaa off* Art aoaaa to psovl4o4 for tbo in to fate a tatb altb mm aa4 water if tlap aoaa la ooataot with tbo iff* of matoxlal tali to to positive* % tMa Z mm if a leak or ^lUago ossut, Si ImmPAo idUai wader theaa olrevBataaoea ahowld to iasirtM # x feoai. t&ifc ube % M& ptim tbo material m tiff hate it Z aaAad that thorewMj ao trothle aroae (81 pod) Ifcodarlok So Sttam SBRN00205B WATER PCB-00051264  r. . * - - * a -vJ.- "_, 18 # ,4J7' *' V> e* & .<= .3 . ,***2>*e>.' If< i.'-tS'-it v: *\ \- r #V* l ___ _ -j; *W ; Medical Research Project Mo MR- ^ ^ y*e .// ' ' . r THE TOXICITY "AND POTENTIAL DANGERS /? INERTZEW i* # * . >.h \ . "/. i * ' . ...... B. \ifr '* . -v ' "Submitted by Vi. F. von Oettingen,1 Ph.D Director Haskell Laboratory of Industrial Toxicology Wilmington, Delaware. _ ' .. "if.* ^snssnoBasBfK^f *"7J8CO. COr** .. V-V WATER_PCB-00051265 Thm Toxicity and Potential Dangers of Xatritin tad R*lat#d Sub's t&aess, Including a Mtthod of Jjuljili for Bjdofieait#*! .................. ........ ......B3lS&Lg\M^ A*v* . . ., _____ , T. T, Ton Osttiagoa, M,D,,# ?h.D. . The toxicological sxptrinsnts on tMi problem ri carried out by Dr J# B* FouIgr uad Dr. A. J* Fleming of tbs Dspartnon- of Toxicology tad tbs pathological studios wsrs ntdo by Dr, I* * Read, Jr of the Dspartneat of Pathology of the Basfcsll L&bor&t' Tha aaterl&l was inrsstigatsd with oral adalnlstratlaa to r* ta, application to the skin of rat*, and in inhalation tzperi aants. The .latter were plumed, in such * way. a to approach as closely as possible the actual conditions encountered in the. as of this material in transformers, in order to eTaluats the aaxi hazard which nay be encountered in its use for this purpose I comparison, additional tests were mace regards the toxic effect froa inhalation of Tapors froa Pyranol and Transforaer. Oil (TTei inghousej In addition, a method was worked but for the deter mination of Xnerteen in air .' Effect of la order to determine the minimal fatal concentration of Xnerteen for rats, 100 animals were given by stos&ch tube slnr doses of Xnerteen, &s indicated in the table. Dose ,fio. of Ho of Time of .4eatb per cent cc./kgo. anlaals dead mortality treated 6 i 1 '. 1.0-1.49 fc6 5 4 4* vithin 5 days 19.H ??I i 1,6-1.99 BBRN003094 i4 10 20 ' '9 5 10 6* Z 5* 2 9* 2 57.6 50.0 60.0 ti ' 2.0-5,49 20 16 16 * S 76.0 WATER_PCB-00051266 s 'la thtss, us la. *uL*quwat sxpsrimeati, an TlI thovtd si pas of discomfort lBacdlstsly following the sdaialatrstioc, lstsr they bscuae depressed tad refused, frequently, wttr and food; within a' feu hour* they beceae teiJc and stuperous, . so that they ttre finally unable to rise. hen this stags wa reached they invariably died* toe of these rats was found to uffer froa albuainuris, oat deTtlopsd tremors of the head nd fore-limbs, end one showed severe hsmorrhuges from the intesti nal tract The table Indicates that with oral cduinis tration the ninimal fatal dose of Inertecn for rati, which Icills 75 per cant of the aniaali within > days, la S*0 to .4 cc# per kilo gram body weight. Upon-- pathological examination of 0 of these auim-ls, those that had died spontaneously showed congestion of the luru:s. Y.hic us'combined vith edeau Mid heu^rrhafe in several instances Tea of the anixuls had mottled gray or yellow livers cad in three instances there res a diffuse pallor with moderate yellowness In 5 out of 6 animals studied cicroscopicully the liver shored narked aid rather extensive hyaline necrosis in the central part of the lobules; the liver cells in this area revealed fatty de generation of the cytoplasm; and in eninali that died 5 and 64 hours after the treatment these cells contained increased nunbera of aitotic figures* In the majority of the animals the mucosa of the intestine v.bS congested and the fecal e-teritl in the -intestines contained' old blood; and in one'instance fresh blood was found in the lov.er third of the ileua, lover Colon, GBRN003095 WATER PCB-00051267 I and sigmoid. mcro*co?io*.lly the of t*o mijyJy pr*aot*d typlo&l fa**orrh*gic erosions of the ueou; another showed heoarrhaglc ar#a 1b the nucaik; and In the rcsjtlninx animals postaortsa changes did sot allow an xact InTestljetioc. In order to folio*' up the toxic effect of Iaerteen on the liver, & croup of 50 white rati ui treated in the suae way wit ilnglt oral doses of 1*15 to 1,20 cc. per kilogram body weight. Six of these were killed 3, 8, and 11 days, respectively, after the administration* ' "Upon p-thologicul examination it was found that two of the 6 animals killed after Z day* had. bloody materials in their stomachs end in 60 per cent of these animals the liver v;as slightly yellow in color uiu the liver cells were large'and coi ti-inod ' numerous mitoses and occasionally there w-s necrosis of cells immediately about the central veins iuilnt.ls killed aft 8 days presented a slight enlargement of the liver with a ques tionable yellowish color, the liver cells were large, those ar the central veins were dark, and occasionally there was soae ftttydegeneration of these cells Eats killed after 11 days showed no important gross pathology* Microscopically, all sec tions showed a slight swelling of the liver cells with occtsic vacuolization o' the cytoplasm# No other' organs shored paths! changes referable to the exposure* # In orcer to study the effect of repeated oral c-drinlstr.-.i of Inerteen, 5 groups of 10 rats each were treated in the fol! Ihg wayi ' 6BRN003096 WATER PCB-00051268 4 Ih first froup rcivd fr 0.S5 to 0,84 ec. ptr tllo for' 5 caastcutlr* daj* Ioa of th dl*d ad 6 #r# miw after the Brd treatJaeot for pathologies. #T*twtloc. Si# second croup us fed doses fro* 0d3 to O.M cc, ptr kilo. ' Two died folio-wring the tod'dose End 6 were ldll#d for mxtopgj after the 5r'd adnlni strati on. In the third croup the dose* rtaced from 1C3 to 1T8 cc* per kilo* On rut died after the 1st, three^ after the tod, and four after the Zrd treataeat, and the regaining anisals tero killed four days after the crd treat- atnt* . . . Upon pathological* exsninr.tion the livers of the rets of th< first, group appeared somewhat lighter than usual and one shoved large yellor; cress; there was i diffuse slid swelling of the liver cells v.ith sone polychrostcit; occasionally the cells sho< soae vacuolar ch-Jiges -Ji the eytoplaan, but in general these changes were cot very severe* In 4 n.ts of the third croup ubi died after 3 treatsents the stoaschs vere dilated with food and in tea of these there v.uc also soae old blood present* iiicro- scopictlly, one rat htc seen infliisaMory ulcers in the fore stonech and another shorc-d bedorrhugie erosions of the pylorus. All shored some fcyperenis. of the liver and in* one rut this v.u3 of Bottled cppeuTence. Hicroscopicully tvo rati.- showed svvellin of the liver cells vith fatty degeneration #of tnose in the cent parts of the liver lobules# tEvo others presented central necro of the liver cells tith hyperplasia c:* the encothelial cells 1b these areas, one shoving in addition, nuaeroua mitotic fir-ires BBRN00S097" WATER PCB-00051269 whs liter calls. Of' 1 ruts which ^ere kill ad 4 dty* foUotiax the. art udxinistration, one had saU.1 uwat of blood in th Ctitrlc content. ' The liters of both Solaris ap se-rec nodsratsl; enlarjd and nieroseopleally there waa a fnraH*ed fvelLiaj or th* liter cells with sooe polychroausia. . Ono rat suffered fro* a fairly general vacuolar degeneration or the liter cells and another presented vacuolar changes in the central part of the lobules* ' In order to compare the toxic effects of Incrteea vith trichlorobensane and ethyl-tetru-penta-chlorobenseae, a croup of 10 rats was given daily doses of trlchiorobengone ranging froa 0#S6 to 0#5B cc* per kilo body weight* One died after, the 1st, four after the tod and four lifter the 3rd Mini&i strut ion, the regaining rat T.au killed 4 days following the erd alia last treataent. ' . It appears, therefore, that daily qosbj of 0,56 to 0.5B cc, per kilo of t-rl chlorobenzene killed DC per cent of the animals' ritb S coses, whereas it -was found that doses of 0.6E to 1*04 ci per kilo of etr:vl-tr-tra-ocnttchlorobenen&. given in the sane way, -killed only 10 per cent, and Inerteer. in doses of 1.hi to 1.7C cc. per kilo, given in the sane way, id.lied DO pex6 cent of the rats. Upon pathological exa~1 nation, animals v.l.ich were treated with trlc?:loroten2e.n0 anc which died & .-ontanc-ously shoved a passive congestion of the lungs tad the liver; the gtontchp v0 ere distended . ith food; in four soae blood tts prtsent `in the ' 6BRNQ03098 WATER PCB-00051270 0 gastric contents and in oa Instance there was a hsaorrhkglc erosion of tb sucosa* In two rata the mu *ko*i irregular Bottling. Lirer 'sections of all nnlaals ahoved necrosis of ' the lirer cells around the castral reins and thuse in the outer parts showed vacuolar degeneration. In rats which died 3 to 4 days after the first treatment there was aoae endothelial hyperplasia in ther,areas, of necrotic lirer cells. One presented an Increase lx^the number of mitotic figures in the lirer cells. . Of the 7 rats treated with Ml^lX^XS^T3^^^XhlOT<>benter#. the one which died spontaneously after tho 3rd dose showed con-. gcation and hemorrhages of the lungs, generalised passive can ' . ' gestlon of the spleen, bone marrovr unu other viscera, distended stonochi aril noderate yellow mottling of the liver, tho liver cells being mildly swollen ni showing fine vacuolar degeneration The animals ridch were killed shpted only a questionable enlarge ment of the- lirer and kidney anu u slight swelling of. the liver cells T.itb occasional racuolur degeneration, .hich*changes were . extremely nild. .' ' grubly less toxic than irlchlorobt/nsene, the ainiaal fatal dose v.lih oral administration. killing 70 per cent of the anicals. hr ini: i: round 3.0 cc. nor kilo rht; r.hereas ethyl-tytra-senta-chlorobcnsene does not iouci r to be neirlv fcs toxic vith oral fcdcinli:trotlon* The ottholo-,,ic;.l chan res observed after oral td.oini stration of Inorteen core: r to he fairly consistent and obvious. Lt-rro doses BBRN003099 . WATER_PCB-00051271 7 hi dlJLMJC&ULjLDLJ^ .B fc 8 S1T .Qf the ti op ' gf -Sht. k Bills,jgugm* ..yithu - vl th ' jjjs^_..&I-xaejenmiilmx-^^ rktd ' after eight days, tnl after eleven davf no definite liver ya^ologL.*^ S* 2T1*ei\\' Pintle large dose? -moir to be sore injurious'than such doses glren In fractions. ' * *. .' ' Ten ahite rst* wt-re treated dally with ta explication of 99 about 0.5 cc. ol Inerteea to the shaved akin of the hack,' pre cautions being taken ta pr-Tent tbsor^tion through the gastro intestinal tract by licking and by inhalation. All rats lost weight during thr experiment but they showed no toxic slims aside f roa a slight restlessness at the'beginning of the ex periment. At the site of the acnlnistrution the skin became dry, thickened and scaled without any fissures being foraed. Sinilar reactions were observed on the human skin especially on the hands, cbweks and forehead# One of the rats clou after 11, and three after 12 treatments, thr regaining being.killed # Hi hours niter the Ibth application. Upon pa tholo.jical examination the liver of til an intis was found u be dirk gray brown in color with mottling on the 6BRN003100 WATER PCB-00051272 surfaea. In those r*t which died spontaneously there uu* Xtitty degeneration of the liter cells with necrosis of those around the central veins and In animals killed at the end of the experiment there was c slid swelling of the liter cells ' with occasional vacuolar degeneruti.m In some. Kicroacopicilly the skin at the Bite of application of A rats showed hyperkera- t ini ration with occasional blister formation, one animal showed perifolliculitis, one. hyperplasia < the eoitheliun rather than hyperkerstin!ration, and in 5 rats there was a nild fibroblarti- proliferation with some round ceil infiltration' in the tmderlyl connective tissue. It appears, therefore, that the contact of Inerteen with the skin does not only cause locr.l reactions such ns drvnesa. thickening uni pc&llng of the skin, but also gvstealc effects a; Indicated by the injurious effect on the liver. Lff(-ct of Inhr.latlon of Vcoors. '' In eruluutinc the toxic effects -of inhalation of vapors liberated frost Inert*.en ut elevated temperatures, attenpts v>erc eaue to reproduce conditions &ore severe then srould be t * ' . eet in the overheating of & transforner* In these experincats rats were exposed in l limited apace of about 1 cubic foot capacity to the vapors of the boiling material which entered directly into the chamber through a hole in the tottos. In each experisent ft ruts wo.re exposed on L5 to G6 occasions for LO ainutej, twice, d-lly, to vapors from Inerteen, Pyranol, or BBRN003101 WATER PCB-00051273 9 Transformer Oil (leatiag'bouse). During this tine thy *h0wwd irritation or tot shin, which' appsirsd to be aost marfcwd on those parts of to# body not protected by hair, mu which per sisted for oat ti af t#r tot exposure. Pyranol appeared to product tht ost effect 1b this respect, followed by Inerteen i,njri- Transformer Oil, in the order given In opposition to toe L rats exposed to Pyranol and Transformer Oil, 3 out of 6 rats exposed to Xnerteetx lost weight* but &o othor toxic Bipu were observed. It is quite possible that rats exposed in this way absorbed sone toxic materiel through the gastro-intestinal tract by .11 clcing the fur during or after the exposure since the sate- rial' had a tendency to condense on the walls of the chaaber and on the surface of toe aninals. The naxisua concentration of Inertaen to which these rats were exposed was detur-inuu as thou* 0.5 nj. per liter of air* * Uoon pathological exaainction of ruts exposed in this way an 14, 25 and 06 occasions to Inerteen, no definite pathological signs could bo observed in the liver or other organs which could be referred to tot. exposure* Two rats treated with 41 exposures to the vapors of Pyruno showed no definite cellular changes in the liver although in one aninal there 'was an inure., sed nunber of aiitotic figures in the liver cells* . . Tv.-o rats exposed ou *4 occasions tu the vapors of Trans feror Oil (riestinghouse) shoved uj definite pathological changes of the internal organs. 6BRN003102 WATER PCB-00051274 10 la rdr to iudyth effects of continue mnTM*- 10 rat* v<ri. axpj4 6 hour* dally on 6 day* a xor eo 'days to cuaccatratloas of 0*08 t(, to U.OB of Irt*c pr liter of air. They ahovad no toxic nor pathological tignj referable to the xuorurt; there tin no definite change* f ' the rod blood corpucls or the hemoglobin* The animal a >re killed day* after StO exporurea* seeted Otg mg. .ef latrJJlt&ILJlXa .S.efd ._r&50 8Urg_ to jeppeentra- tlons of 0*05 to 0,09 ar. per liter nir cause a definite- toxic effect on the liver* - ` . ' *' . Deterainstion of Concentrations of Inertoen In the J-lr. In order to determine the concentration of Inerteen vapors in the air, the following nephelometric cothod was.worked out, after several other procedures had bees considered, A definite voluae of fair to be tested is drara tt a rate of about 1 liter every 4 Blnutes through t test tube containing cc. of ethyl alcohol, istersed in cry ice-acetone mixture in order to prevent the evaporation of the alcohol At the end of the stapling 1 cc. of. the alcohol v.aa nixed vith 10 cc. of dis tilled rater and the resulting turbidity was set sured with & photo electric cell, usin;. t. sodiun vapor lamp us the source of light. '' * The turbidity of unknown staples was compared to the ' BBRM003103 WATER PCB-00051275 These experlse&ts kow that the cmcmirtUoa* f 2urti in iir dtcr#8e rapidly with the distance fro, the ouret *f their proAict,# . la order to study variations of the concentration* over s period of time and with different teaperutures, a curmt of 10 liter* per alwate of air us passed over the surface of lar- teen of about 10 square laches, contained in a flask and thenoe into a bell Jar. Samples were taken froa the jar`at various intervals after the flow was started and with various teaperature The following concentrations ware detersinedi . . Tine of Concentration of sampling trichlorobenzene in hour* . in mg* per liter Temperature of trichlorobenzene in flask ' C. * .f ` 6 1 4 1 ' . . Trichlorobenzene 0.29 0.51 0.60 1.68 1.70 1,90 ' Inerteea ' E3 2 28 bO 50 . 90 * . 6 0.&8* ` 5 * . ' This tabulation shows that the deterainatlons marie -at ' feC* and with the 6 hour sample were alaost the sane for trichlorobonxene (0,60 eg per liter) and Inerteea (0.58 ng* per liter). This suggests the possibility that the bulk of the vapors liVyrated froa Inertean at this .temperature nay be ' trichlorobenseaej so that the hazards froa inhalation of Iner- teen vapors are identical r.ith those froa the inhalation of ' GBRNOOS104 WATER PCB-00051276 trIeM.robms* to order to coafim thla, Mi cc. or Inarteen vara aubdttcd to fractional distil 1 itioc t,h*i foiloriag revolts w obtilnarti Fra c Hoc 1 8 4 EesidsM Tacparatura of dietlllatian *C. 240 40-254 254-280 80-800 above WO Toluca caU*ct*d ee . sb 48 45 SO 180 Specific BoiliM Gravity Point *8 of fraction 1,488 1.478 1*405 1*877 1.892 808-210 40 69 Since ,.the opocific gr&Tity of trichlorobenzene is 1*466 . aci the boiling point 0BC*-219*C*, it is evident that up to 240C. the Tapors consist exclusively of trichlorobenzene and that for this reason the Lbove statement Is justified, naselr. thfet far iao3t~ conditions the hazards froa vcoors of Inerteea. t-.T's identical rrlth those froa trlchlorobenzene* ' ' ' Beaune. .. The experiments discussed in this report show that vith oral administration Xnerteen is considerably less toxic than tri chlorobenzene, .the ainiaal futal dose Killing froa 70 to . /' 75 per cent of t, he rats being around 30 cc. per kilogram body weight and 1.4 to 1*B per kilogram body weight, respectively* Fatal doses rill cause passive congestion of all viscera, ex tensive degeneration of the liver, und ulceration of the gas tri ( mucosa* tfith sublethal doses these effects ere loss severe end there Is evidence that they rill heal then no further exposure occurs* . SBRNQQ3105 WATER_PCB-00051277 Continued application of Inertten to the tkln of nti end humans causes dryness of the tJdA, thickening tnd scaling; end the observations wide In.rats indicate that sufficient e quantities cay be absorbed through the skin to produce injuri ous effects on the liver* , Repeated inhalation for short periods of concentrations of 0*5 mg. of Inerteen vapors per liter of air, or repeated. Inhalation for 8 hours of concentrations of 0*05 to 0*09 mg* per liter of air causes no definite injurious effects in rats* Vapors liberated from boiling Pyranol, Inerteen, and Irons- former Oil (TTestinghouse) are Irritant end the Irritant action decreases froa Pyranol to Transformer Oil (Vestingbouse), In erteen being Intermediate in this respect* It has boon shorn that Tapors liberates froa Inerteen under conditions approaching those as night be encountered in transformers consist mainly of trichlorobensene. ' . a simple method for the determination of Inerteen (tri- chlorobeasone). Tapors In air is given* If 10 liters of air are dretn at a rate of about 1 liter every minutes through & test tube containing 1 cc* of ethyl alcohol, cooled In dry ice or In an let' salt mixture, and the alcohol, is then poured care fully on the surface of n few cubic .'centimeters of water in a test tube", a ring of turbidity is produced .If the concentra tion of Inerteen (trichlorobensene) is over 0*03 tag. per liter of air. If under these conditions a white ring Is produced, 6BRN003106 WATER_PCB-00051278 the air tested should be regarded rith suspielcm hnd should be improved by more effective reoiUiUim*. .. . . It was found that the concentration of Inerteen (trl- chlorobensent) in a closed fp&c* 14 inches shore the surface ; of boiling Inerteen is 4.5 mg, per liter and in an .op pac 5 inches aboTe the surface of boiling Inerteen is 0,56 ag* per liter, and when the temperature in a transformer, standing in a closed rooa (mult), rises to B0C. the air nay contain 1,8 mg per liter of sir* . Proa 'the s-uin&l experiments^reported, it appears that concentrations below 0,05 fig per liter of air will cause *no ^ _ i" i i # toxic signs or synptons even with continued exposure Regards preventive aeesures. the following nay be suggests ` It appear-' to be cf paramount inport:nce thi.t the conttai nt tion of the air be reduced is concentrations below 0.05 mg pe liter of air by adequate forced ventilation tt the site of the ' production of such vapors, ' Greatest personal hygiene is not less icpsrtant# Contsni- nation of the skin should be cToided by wearing proper protectiv garments. such as gloves, caps, and coveralls* In case of cccide or tith exposure to higher concentrations of and above 0#2 eg p liter, respirators or open air masks should, be worn. The akin shoal'd be kept iaxaculutely clean ana ointments such as lanolin or Aquafor should be applied to the skin after washing the hands la view cl - the hepatotoxic action of this compound, indi- riduals suffering from injuries of the liver, syphilis, and hear / BBRN003107 WATER PCB-00051279 ihould bt xcludtd fra* operations in vhich I* hndld* ' . . Vorttrs hinrtllng Inrt*u or *ith frequent exposure to It* vapor* should `have periodic enril nations, special attention should be paid to their nutritional caaciti# ind tht coalition of the liver m.j be checked by aeteralnln,, the Icteric Index la the blood, tal the urobilin and urobilinogen excretion in the urine* . `. Regards the trectaent of toxic effects produced by exposur to Inerteea, it appears tdrisable to Increase the resistance of the liver by carbohydrate diet; i4mIMjtrtion of glucose and insulin may be advisable, ana duodenal lavage with nagnesiua sulfate aay be tried* Local irritation of the skin produced by Inerteea should be treated i.ith blend ointaents after the toxic, caterial has been reaoved by intensive vasiiin,; and scrubbing. In case Inerteea has been taken by noutb, the- toxic naterie.1 should be removed froa tha stoaach by eaetics ouch ts soap water or maturd'fitter, and this should be followed by gastric lavage with a suspension of activated charcoal in water and saline . cathartics such as Epson salts. '' co28 38 4* ' BBRN003108 WATER PCB-00051280 THE. MIICQWQ1 OF IMMTWM AMD eb. STAfcCXE IHCLUDIVG 1 UTIiiOv vF AMAL1BIB ft? a . vC t* r_* . r ' A* J. TlMlAf, H. fi ' The Toxicology of Xxrta m laves tigs ted by oral administration, i/cln application, and inhalation experiments in rat* In the latter an attempt was sad a to investigate the substance in a way relative to ita uae in tranaforaera and to deterrine toe saxlsua hazard that sight ariaa ahould in* substance be used for that purpose* The einlaus fatal dose was determined by oral ednimiatration and toe affect of repeated oral dosea was a tailed and compared w-lth toe effect of aiailer doses of trlchlorobenaene and a thylts^i^panta-chlorobenzene. A xetood cf air analysis' for the halogeaated hydrocarbons was derised and air analyses were Bade to determine the con centrations of Inerteen in to# air near open and closed contain ers when the substance was heated to various teaperatures end whan samples were taiien at various distances fron the source. A statement of the problems incident to the toxicology of Inertcen and the answers to these probless will be found in the conclusions and sunnary at the end of the paper (1), Single Doaea The substance was given in single graced doses to severe! groups of rets to detercine the ninlnun fatal dose cnnnAfii 300021 WATER PCB-00051281 t# t 8S8So t 01 rrw vr to ae & cr S03 O r*. ayi c V c &> Ol * g 1 * o-.* cc. H f* I B a t g & -*> o n & C! t8 o> a 1 9 *< o a C tHjPrC p; Ht= ^3 tr. o* o o -4 H tc KO *0o <*f -< r0* c * o o O - t* . to -> a H* ft (nonari/ 30002 o WATER PCB-00051282 _ Ths rMulU r eonvaaiatiy tabulated in tabl l. ' llLttt-i ' Jlm not#d, ddi# of & to 8,5 ee. pr kilograr gmv# a 75 p*r etnt mortality. Twenty-turo of till* croup f in<nii vir *ut*psl*d, Another group of 83 ravs wms glTcn <p;i oral dostf ranfInc froc 1,15 to 10 cc. par kilogr**, Six of thes# vara killed Z day* after traataant and axaailnad by ths pathology dapar^ant for potalbla llTer daaa|t, fix vara till ad 6 days after traataant and xamlnsd for possible kidney change and 6 vara klUad 11 days after trsataent, and axaninad for potsibla brain dauga* K \ ' U) Xa' Thirty rats were divided into groups of ten. The first group received Iron 0,55 to 0.56 cc. per kilogram for Z treatments, Iona died and 5 vere killed for autopsy within 4 hours after the 3rd traetsent. la the second group, the dosage ranged, fron 0.65 to 0.66 cc per kilogram. Two died after the second treatsent and 5 were killed for autopsy 4 hours after the last treetceht. In the third group the dosage ranged from 1.23 to 1.76 cc. per kilo. One died after 1 treatment, 3 died after treatments, and 4 died after 'tee 3rd treatsent. All animals in this lest group vere autopsied within 4 hrs of the last treatsent. Ir/'general all rats behaved tee sene following oral ># administration of Xnerteen* They proceeded at- once to eat as if to allay the discomfort caused by the substance. Following this they became depressed and would not eat and often would net rnon^?) 300023 WATER PCB-00051283 drink ImJqiii ans stupor ftntraHy rupirvta#4 wittin fn houn until the animal* ..could no longer riae for food *** areter IiQuidf w%t9 taken, howewar, 1 * edninis tr ated in/4 for a few alnutes following ad a4.r.l strati on the anlaal* parked op a bit The improvement wai only inaiporaxy tad the oattosa, when they bad thus far proirus^, wma invariably fatal. One animal ihowtd an albuminuria (tested post mortem) Mid on* de veloped tremors of to# head,. and front limbs. 0n had severe hemorrhegas fron toe ractuc and toe autopay indicated tha bleeding nt from the lower and of tha asall bowel. Comparison of Inertaan with tr 1 chi oro bans ana and Bthyl-tetra-pfntc-chlgx&bftasftllf...... ............ ' 1 group of 10 animals was given repeated doses of trlchlorobenzane ringing froa 0.56 to 0.68 cc per kilogroe. One died after toe lat treatment, 4 died aftar the nd, and 4 died after the 3rd The remaining animal was killed 4 day* after the 3rd and last treatment. All enlaals were autopsied. i Similar groups were treated with Inerteen taad ethyl-tetra-pente chlorobenzene and the following noted! Daily doses of 1.23 to 1.76 cc per kilogran of Inertaan killed 60 per cant of the anlaals, when 5 doses were given, while dully coses of 0.36 to 0.56 cc. per kilogran of trichlorobenzene killed 90 per cent of the animals with 3 doses On the other hand daily doses of etkyi-tetra-penta-chlorobenxen ranging from 0.62 to 1,04 cc per kilogram*killed 1 rat in a group of 10 with Z doses. . . Conclusion! fnnn&H4 T/.e Eir.itnii fatal dot-e of Inarteea appeers to be ' 300024 WATER PCB-00051284 around 2.0 ec. par kHogrj9 d^ses of X&artaas vra fatal ta oneactrations b#tw@n O.SS and 1.71 ec. pr tilotm, while repeated doses of irichierotmMan* vin fatal in eae. tratiosj betwweo 0.#6 aad 0iS ae. per kllacm, p#at*-<Bh20TebnJt does not appaar to ba muIj *o Uxie fey ral adalniatration* flalf a ubie centimeter f Xncrteen ii applied dail; to the shaved backs of 10 rati by ceans of a a mail glass cup filled with a piece of cotton wool soaked in the substance. The whole ni itrappad to tha animals with adhtsive tape. On* rat diad after ll treatments. Thraa dlad aftar 13 traataenti and th retaining salads wara killed for autopiy 14 hour* after tne 151 treatment. AH rats lost weight during the wxperiaent, but out side of a slight restlessness at the beginning of the experiment showed no ether signs. The Inerteen actad locally on the akin, producing an excessive dryneai with aubsequent thickening and scaling without any fissures being foraed. Tha sane affects wer noted on the human skin with respect .to the drying and slight scaling and were cost notable on the hands, cheeks and forehead. An attaspt was eada to reproduce conditions core sever than would be ret in the overheating of a transformer and expos ing rats to these conditions for 0 cinutes twice a day. 300023 WATER_PCB-00051285  tha afortfeiag-AA4rm> npriiuti i to of *boux 1 uMc_foot aapocit7# in one eorner of which i tot inlet fra a |lui flask containing the tubs tanee balng inTtatigatad, Xn trtem, fyrnaol r traWr#r oil (Waatiaghouji) r9 pilc^ to tha tLook tad brought to a tell Sw rata vara *>>* la tho box uyi allewd to roailB for 10 ainutaa, during which tiaa a ftn*rtii*td itching of to* skin appu*#d which wi t *xk#d in to* part* of tho body not protected by hair Tha itefainess pariiated for aooetiae after tha animals vara remove* from tha box* fyranol aaasad to product tot coat affact to thla respeet with Inertean and Tranjforaar ail foHovinc in tot ordtr mad, Three out of 6 of tot Inertean treated rata lot weight, while toe Pyrtnol and Transformer oil treated rata fair weight ( rats only in each of toe last too groups) It la quit* possible that these anlaala ingested a considerable enoun of these aufcstances by licking their fur after resoval froc toe X box. lo narked change in respirations were noted* although the anlsala one* or twice breathed faster than norsel and occasion ally tha axtrasities were slightly blue At autopsy bo gross pathology was noted. The naxiaua concentration of Inertean to which these rats ware exposed was about 0,5 mg per liter Tha box was aired between readings, but not washed out. 0 With Inertean too rats received 8 treatments, two # received .J5 treatments and too received 66 treatments. With Pyranol two rats received <2 treatments and with Transformer Oil too rats received 44 treatments 300020 WATER PCB-00051286 6- . A group of. ton riti m for to 4*j tig^t 41 . hour* par day to aaaeratritioaj of Zaertoen la the tjj. from 0o0S to 0,09 m ftr 111 nt tin killed for petaalegy witMn fro day* following toa S5th dty of light of tol* group gained weight, on* loit weight tad mi showed no changa, 71w* *hovd a flight 4rp In th* r*4 blod count, three showed an Increased red blood fount and two shoved no chang*. The ehmagti in th* haawglobln paralleled tot in th rd blo^d eount* r 9 c & r bon . .Considerable difficulty was experienced in ostaining a satisfactory tood of air analysis for these suostancei and a nephelometric cethod was finally adopted. In this, a difinit* volume of the air to b* tested vas drawn at t rate of about 1 liter every four minutes through 5 cc. of ethyl alconol cooled la a cry ice-acetone mixture. The latter being necessary to prevent evaporation of the alcohol. One cubic centimeter of toe alcohol was toen nixed with 10 cc of distilled water and to resultant turbidity measured with a photo electric cell, using a sodium vapour lamp as a source of light The turbidity of un known staples, was cospared to the turbidity produced by known standards mad* up of trichlorobenzene and ethyl alcohol, Inis cithod gave a satisfactory range of readings for concentrations varying fron 0.30 eg. per liter to 0.03 mg/ per liter which, when the original dilutions were taken into account, was suffi cient to detect a* low as 0.03 mg* per liter of Inerteen in the sir tested. The method is not specific for the various nenbera of the halogen*ted hydrocar Dons. COOO^fV? 30002/ WATER PCB-00051287 lartic. . . " the effect ef aryttg the diit*act at which iu^Iu ware taxen froa * cLoiti p*ct orr boiling lart4a wm deter- mlntd wltt Xh fellovtts f*uii#s Miaae latim 14 Cooeeatratloa 4.50 to 1.* 19" ' 1.14 1.14 lirilaxly the %fttct of warylng the distance at which iasplas were taken OTer an optn beaaer cf boiling Inertee was deternined with tht following reaulti Distance Concentration I 0.56 10 0.4S 15 O'U to 0@4 concentrations fall off rapidly and if any coolins surface is imt* the Inerteen and no air currents are blow ing oTtr the surface of the Inerteen, there if ouch leas chance of any appreciable aaount escaping Into the atsosphere as free a container like %ramfomer. . C000&?>8 ' Paneling at Various fise.latjjxi.ls_ and ..Teifferajureg. Mr at 10 liters per minute was passed'over a surf ace of Xnerteen (about 10 *c. inches) contained in a flack and thence into a bell jar" Samples were taken froc the bell ^nnnoo WATER PCB-00051288 Jtr at various intervals after the air flaw sma a tar tad and under various conditions of temperature. Til* of CoaemtriUoa of Temperature of Sampling . IriohLorbasn* Triahlorobenjunt At M*C. 1/ i bmr 0.19 m * 0.81 m 0.80 u M I0C. 1 i.ea to 4 1.70 to At 90C. 1 1.90 0 Inartaan at 0C, 6 0.&S tz Trem the foregoing it will be noted that toe 6 hour staple with trichlorobanzane at 3C gives alaost the sane con centretion (0*60 ag, par liter) as did tha six hour lample with Laertee:; at 3C, (0.58 ag, per liter) This suggests the poas bility that toe bulk of the stuff coning off the Xnarteen at that temperature say be tricklorobeasese and that the hazard* o In6rteen Bay thus b tha hazards of trichlorobanzane fraction al distillation of about 335 ec. of Inerteen was carried out Is a distilling flask with a 300C thersoseter reaching to the level of the side are. The distilling flask was attached to a Liebig condenser end e collecting flask Samples were collects over temperature ranges from 4DC to 300C, (The temperature reco'rded being that of the vapor* .around toe .thernoneter bulb Tne distance between the bulb and the surface of'toe liquid vac about 6 inches. Although the liquid boiled vigorously several minutes elapsed before the'vapor reached the bulb). The bcilsnnnoQ WATER PCB-00051289 lag poiat and pacific fxivlty wj nitrurtd for mea fraction ooUiet*4# Temperature of Bo 11 live Point Fraction Condensing Liquid Fraction Bmo, Grav. I, Mo. *c. 1 5 4 Residue MO * C40-454 54-160 . 83-200 .Above 200 B06 - 119 IU ' 140 MB l*4tB 1,476 1,492 1,877 1.59E 118 45 48 m 110 .Fraction #1 m probably triehloroberueae (6pci- flc gravity 1.466, boiling point 06 - *19C.), In investigating the toxicology of Inerteen answers to the folioring questions were fought and are 'here given es far as posslolt, * (1). What i the composition of the Taper* liberate Iron Inerteen at a saxlaus working teapereture of 8DC# Trichlorobenzene only. v () What is the m&xlBua concentration of 'toil fraction to which workers sight possibly be exposed, . (a) In a closed space 14* over boiling Inertee: 4.5 ng# per liter. . OWUUGO (b) In an open space 5* over boiling Inerteen # 0.56 eg. per liter. ' (3), *hat eight be toe at* Inrun concentration in a room where transformers are placed when toe tespenture of the transformers- are 90C, and the air has a chance to get eatu- snnn :<n WATER PCB-00051290 _ 1.1 m Pr Utir. (4) Vhat li a safe aemniritlon n ahorn by animal azparimasta* Coaildfring the hazard i 4u, wmd#r rdinary working conditions to iricfalorobtaztot %on%9 . (a) Fro* irichlorobamimt data previously btmlaed, #0M at. pr liter. ' (b) froa Inerteen data- - ,048 mg.per liter ' The last figure ha* been verified by exposing rata for 8 hour* per day to such concentrations over a period of i**#iks, . (5) 1* thar a S4sple test that alii detect con* centratlons of Znartaan below .048 a*, ptr liter, s leae If 10 liters of air art drawn at a . ratt of about one liter every cinutes through 1 cc. of ethyl alcohol (cooled in i dry let or an ice salt mixture) and the alcohol poured over the surface of a few cc. of distilled water in a test tube a ring of turbidity will be produced if the . concentration is over 0.02 mg. per liter If a ring is produced, the air.tested should be regarded with suspicion and increased ventilation provided. *# (6). that is the minimum fatal dote orally! 5 to 5.5 cc par kilogram. : - 7m (7) . Is there any shin hazard? Constant exposure makes the akin excessively dry, and long continued^jx^osure WATER PCB-00051291 radr proa* ufotptlbl* to too** dtrMtoa wai chart proat to exist Is, ^iissifily dry ifcl&j. 8/&8/M fJ4Prwf** r- /> <-* * '* 300032 WATER PCB-00051292 - Tha SLffee t of art*z fcad Imrtl JUlatwd teb*tj*ncn ffrqa th* Whit* Eat*_______ ` 1. I. Uid, Jr,, *& In*rt*a, aixtur* of irichlor^btM, #thjrl-ttr*pmu-ctlarebwiici imd chioriMi^d dlphocjl, was di*ini*tr*d to whit* rat* orally, by kl& wppliestioc, tad by lnhslatioc. In addition *T*ral tniatli **r* txpottd to trichlorobaxwn* anJ tthjrl tetra-ptatwchlorobtaiant tp*rfttily Two rata were *ploywd to itudy the effects of inhalation of t conpound taora as Pyraaol, and two other animals were ex posed to vapors of teatinghoui* Transforaer Oil* Inertetn OrsI administration. Tcenty-four white rats received e ingle doses from 1L1 to 5*44 cc. per kilogram of body weight Follot.lnj treatment death occurred in LG to 54 hours. One died Immediately follow ing treatment, the eeterisl haring beta partly Introduced into the lungs. Gross Pathology. Lung si *ost of the animals that died show congestion v ith or rithout edenn ui: heaorrhage* EXHIBIT NO_____ mriOaf.3 Liver: Ten rata have mottled gray or yellow livers, ihree animals show l diffuse pallor with aoderste yellowness, '# Gtoaachi In 17 rats the stoanch contains blood. Kine of these present grossly visible erosions of the pylorus Intestine! In the majority of the an 1 sals the fecal c-ter contains old blood In one anlnal killed 54 hours aft treatment the lower third of the ilrua contains bloody a; terial* There is congestion of the bucoso. The lower colon tno signoid also contain bloody material* 300033 o< WATER PCB-00051293 t Mlcrgwoslc Patholocr. ' ill rat* iPi examined histologically* Linn Fit* ahos. wreia anu. rsthar rncilTt fayaHn necros: in the central part of tie lobules. The liver celle mbc thm area* present fatty defeneration of the cytoplasm. la two animals living ft and 54 hour* after treatment tl are increased numbers of mitotic figures. Stomach! Two animals pre'aent typical hemorrhagic erosions c the mucosa, another has hemorrhagic areas in the nucosa. The rest of the animals show post mortaa change which partially masks preceding pathology* The reaalnder of the Tlscera presents no chances that are thought to be of importance* Eighteen rats were given l dose of 1.15 to 1,20 cc. per kilogram body veight. Six of these animals sere killed fc days after treatment. Six anis&ls %re killed 6 days after treatment Six animals were killed 11 days after treatment. Gross Pathology. Stomochi In of the 6 animals killed after L dayb there is bloody material in toe stonoch. Lireri In half of the animals killed after S days the lire are slightly pale yellov in color. Those killed after days present slight enlargement of the liver with a ques tionable yellowish color* Rats killed after 11 days present no important nothology. Mieroflee^ie Pathology* Liver! Exposure 5 days. The liver cells are large v.itfa numerous mitoses. Occasionally there is necrosis of cells immediately about the central veins. Exposure 6 days. The liver cells are large. . Those . about the central veins are dark. Only occasional fatty degeneration is seen. Exposure 11 days All of the sections- show slight swelling of liver cells \.lth very occasional vacuoliiati of liver cell cytoplasm. None of the other viscera present pathology of importance to the experiment. 3 0003 J. WATER PCB-00051294 m i i . TwMty^ooe rati rootived multiple triUcti by %outfa.. The *-*ount of a single dost Tariea frsa 0*40 to 1,75 cc, par kilogrui body lfht. The aalmls studied histologically ri Group 1 4 rats, 1,84-1.75 cc per jdlograx. Di#d after Z diJJy treatments. 0*onp L. t rt-ta, l.f-l.Cb cc par kilogram. Killed 4 daji after 5.daily traitautii Croup 2 ft rata, 0,4-0*48 cc, par kilogram. killed 4 day* ' after 5 daily treatment*. GrQej,_2_z&nlpjsf, Group 1, Stomach: All are dilcted tith food . In there is aoae old blood present in the content Liven All preaent aoae fayporeaia. In 1 the surface has a mottled appearance. Croup L Stomach: One unlatl has a small amount of tiooc in toe gastric content# Lifers Both present moderate enlargement. Group 5 Lifers Use livers appear somewhat lighter than usual In one there are large yellow areas Microscopic P?-tholo.rr Group 1 Stosachi One rat hag small Inflammatory ulcers of the fore-stomach* another presents'heacrrhtsic erosions of toe pylorus. Liver* Two animals shot swelling oi liver cells with fatty degeneration of cells in the cent? part of the liver lobules. Two animals prese central necrosis of liver cells with hyp&rpla of the endothelial cell! in these areas. In of these animals numerous mitotic figures are found in liver cells. Group 2. rnnnscrz I i MII l-r*o Liver! Ther^ is l.generalized swelling, of liver cells with soae polychrosasia.- In one rat th is n fairly generalized vacuolar degeneration liver cells. The other presents vacuolar chn: in the central part of the lobules. 300035 WATER PCB-00051295 4 Group 5 ~ Livar: There is 'u dlf fuaa, *2d *f Liver etna with *o* u&tiiii in utility. wcc*3lqal liter etUi pre*ot cuoIat change la the cjtopLtm, Pithaloo' of aH of the udsdi 1* ml crni. teigagnto The pathology resulting froo oral Ln*etion of Xnerteen ii fairly consistent and obvioua. ` Large doses which are lethal In one or two days cauae a terainel passive congestion of viscera, extensive degeneration of the liter, v.ith necrosis about the central reins ana local ulcerations o: the gastric bucose. If sub-lethal coses are given and the a&ia&Is sacrificed it different tine intervals, the resulting pathology 1st Z days - gc.stric irritation, hepatic degeneration and active regeneration* 6 cays - mild degenerative changes in the liver with foci of regenerated liver cells 11 days - indefinite liver pathology. ' In the group of animals gives repeated oral treatments, those that dies present gastric ulceration and hepatic degenera tion similar %j those receiving & single lethal dose *wo ruts surviving 5 successive treatments sLov. similar changes but to & less severe degree. The croup of rats receiving c daily doses of Inerteea, the total of '.-hich amounted to lethal or sub-lethal level, presents aild to moderate degenerative chances in the liver Other visceral pathology hue not been included because it is considered to be coincidental in character. It nay be neno n n n o r* WATER PCB-00051296  Sever. rets received about 0*5 ec. of Iartn dally to the ihirei aJcla of the bach. Qus vat protoctod by a jiui rtn# and adhesive tape to preTtai licking. Oae aninal di*d afi*r 11 treatments, the reat were killed after 15 applica tions* ' Liven All of the livers are dark gray brown in color with Bottling of the aurfaca* Bkini Hu gross change is observed excent in the that died. Here the area of application is oft and necrotic in appearance. This anlaud also presents pulmonary congestion# Hcg.ajjAilg,,,Ekthaljaiy The animal that died presentsi Liven Fatty degeneration of liver cells vlth necrosis of those about the central veins Skin? Hyperkerutiniration with blister formation and leucocytic infiltration. There ;-re die inflasnatory changes in the underlying connective tissue. In the six anlult killed there isi Liven Mild awelling of the liver cells in all of the animals with occasional vacuolar degeneration in some of the liver cella c;nnn^ft7 Skim There is hyperkerctiniration in 4 rats with oc casional blister formation Bair follicles are increased in number in three and decreased in one. One aniotl alto presents peri-folliculitis. One of the tniJBLls has a hyperplasia of the epithelium rather than kyperkeratinlzotion. In 5 rata there is did fibroblastic proliferation with some round - cell infiltration in the underlying connective tissue There is no question that skin application produces ioee absorption o; the cateriel. In one animal this was sufficient to produce death Lincc there is injury0 to the akin the degree of absorption nay r.ell depend on the amount of dasi-*Q-0-^ ^ WATER_PCB-00051297 !< Group 1, Two rats were girm maximum cuoceatra tiaaj of rmpora i of Insrtemn (about 0*4 mg. per liter) with czDosore tvics daily for 0 minutes eh. The aalaals sr ttHtd l days aftar 14 trmatmmnts* Group . Two rata were given vapor* containing about 0.4 mg. per liter. Thia m givan twloe dally for M truv> ) manta. One `died, the the- animal caa killed. (i Group 5. Two rats recaived two daily exposure* for 0 aimitea ach of vapors comtwining about 0*4 mg. per liter. These animals were kill ad after 66 treatment*. j Group 4. Ten rata received 8 hour erporurea 5 day* a week of ' 1i vapors containing an average of 0.057 and 0.061 age par liter. These an1 mils were killed after 0 treat ments* The animal that died 1b Group 2 presents b coincidental infection* In the rest of the anltaila there trr tape rorn Infesta tions of the liver and two nts hive puluouury infections No pathology of importance is sera. Mlcr QJLC o^lgJfcllljl23L Croup 1 lo stri)dng pathology. One animal presents bronchitis* ' Croup In the animal that died the bone marrow, liver <uji& spleen suggest coincidental infection* Group Z, The liver ahows questionable swelling of cells Fat stains arc entirely negative for degenerative changes* Group 4. * Lungs Bronchitis or bronchopneumonia or both i re found in < animal* spleens Five rats present fairly ntr^eu erythro- phagla. . *. Font, harrori In those ar.inc.ls that have pulaomr infections there is hyperplasia of-cells of the eranultr series. CflftOiJbfl 300038 WATER PCB-00051298 hile th Lacldaae* of Im* laf^ctloos la hi yK ^ ruts xusod to XarteB by Inhalatioo of vapors, it coast be said that this 1* dirscUj du to XasrtQ. Tbre is ao definite llTtp ma- no other pstholocy thet 1* of soy signifioanes. toaua Oral sdaialstratioo of Insrtssn msy produce local gastric ulesrstion tad hepatic dsgsasrstion particularly of the central part of the lobule*. Ctstr^llsod passive congestion is produced si a terminal event in lethal cases* Folioring single oral treatments there is evidence of hepatic regeneration in about k to days milch becosei complete in about 10 days to k veeks. Bkin application results in injury to the skin end absorp tion of Inerteen, the aaount of absorption presumably depending on the auount of cutaneous damage* . Inhalation of Inerteen products no definite pathology of the viscera* Trichlorobentene Nine rats received daily oral tre-ataents viih trichloroben2ene, the individual dose Tidying iron 0.c6 to 0.59 cc. per kilogram body veight* Two rats died overnight after 1 treetaent; tro died 4 hoars after the 2nd' treetaentj one died over night after 2 treat-eats; one died 4 hours after 2 treatments; rwwvsRQ ' 300030 WATER PCB-00051299 8 two diad vt might After 2 irsatstata; and one ret u irini< 4 4aj After 3 trautaants# Qr^sg Patholorv. In ell animals that died there is passive eaageetian of the luaia end liver# Stomachs In all animals th* atoaach is ovrditnd*d alth food In four there is soae blood present in the geit content* Liven In addition to passive congestion tv>o rata shot an ' irregular yellow aottllag* Liven All aections reveal necrosis of liver cells about the centr-1 veins of the lobules, the liver cells ia the outer part shot-. vacuolcr degeneration. If decth occurred curly hyperemia is alio severe When the animal died 5 or 4 days after the first treatment, endothelibl hyperplotiu ia seen in the areas of ne crotic liver cells One anisud. presents increase in number of mitotic figures in liver cells. Stos-chs In one anim.l there is hemorrhagic erosion of the mucosa* Kthyl-tetra-oenta-chlorobentene ' Seven rats received dully doses frou 0.62 to 0*94 cc. per kilogram body v. eight of ethyl-tutra-penta-chlorobenzene. One rat receiving the highest uost died after the 3rd treatment. Six ruts >ere killed 4 days after Z treatments# Prosi Pathology. ' She animal that died reveals! # Livers -jclcrate yellov, Bottling# Stomachs ^ilatoJ \.ith food# Lungsi Congestion i-nd hemorrhage# rnnn M 70 ' 300010 WATER PCB-00051300 Tba fix rat* idJUea p?aeat qmestlammble eaxlargemeat of fcl dnejT and liver. Mlxaifla&fi-iifralag> l the rat that dimd there l mild wihh; 0f livtr etll with fine vacuolar degeneration. Generalised pmiTi congestion of lung, apleoa, boat marrow and other viscera. In the animals that wars killad there Ii . Liven Slight twilling of liver etlls with occasional vacuoltr degeneration. The change are extremely mild. ' fiflaat&l The hepatic change5 following trichlorober.aene are Identical with those seen after Inert .an* thyl-t*tre-pentachlorobensene produced relatively little oorphologic.l change in the seven animals examined. The one animal that died pre sents aainly generalited visceral passive congestion with only mild degenerative changes In the liver. . mssl Two rats were exposed to vapors from distillation of Pyr&nol Exposura v*s given twice a day for 20 minutes. Forty-one treatsents were given. Groes Pathology. . Bo definite pathology is seen. silerdseasle Pathology. ' r,r, : ' ' i ' )o /` In one animal there are increased numbers of mitotic figures in the liver. The liver, however, presents no defi nite cellular change. 30004 WATER_PCB-00051301 UlM&UBULJJUL Swa rats were xpo#d to vapors of dlatlil<> Trm>farmer OH# This u {Iran 0 minutes, twice dally for 44 triaUnti. fimiJCftSbalVT* lo definite pathology it seen* ^ *l9rg|ggglg fittlllgpr* ' Umff Is on* animal seTeral of the bronchioles contain macrophages filled with eosin staining granules or nail refructile droplets* Ma striking pathology is obserred in either animal* o li& * c6 4* 300042 WATER_PCB-00051302 * February 1** 1950 Dr. Louis W. Spolyar, Director Division of Industrial Hygiene Indiana State Board of Health 1098 '.feat Michigan Street Indianapolis 7# Indiana ' Dear Dr. Spolyar: I enclose an application bulletin on our Arodors. Cn page 19 there la a summary of almost all our toxicology Information on this compound. If the case you refer to Is In Brazil, Indiana, our company has had some contact with the problem; Thlg--particular Installation used a temporary heat transfer system, and thus did not make tJuTTnatanation air tight. This Is contrary to our expressed Instructions when Aroclor Is to be used at elevated temperatures. Upon hearing of the Illness, one of our development engineers went to the plant and gave his recommendations, and then I called the plant physician to try to obtain some Idea of what the Illnesses were. As far as I could determine, two men suffered from gastrointestinal upset. I suspected . the possibility that the* Aroclor fumes might have caused liver damage, but was unable to obtain this Information over the phone. X was also unable to contact the employee's physician. The toxicology of Aroolors Is somewhat confused. The experimental work was done by Dr. Drinker at Harvard about 12 years ago, and was done in connection with chlorinated naphthylene, chlorinated diphenyl, and chlorinated diphenyl high boiler. Both of .these last two are Aroolors. In the particular work at Harvard, Dr. Drinker found that Aroclor 1263, which means ihenyl chlorinated to 68^, was of low toxicity. The confusion existed In his findings that Aroclor 125* which Is the diphenyl chlorinated to only 5*.* was considerably more toxic on inhalation. We did not supply him with this material, and I was never convinced that some error might not have been made in the sample. .. At any rate, we have advised protection against all Aroclor fumes when an elevated temperature Is used. I will appreciate It If you will let me know the result of your investigation. If one la to be made. Very truly yours BEKirg B CCi Mr. 'Paul Benlgnua . St.. Louis i. Emmet Kelly, H.E Jbdloal Director ,4453 900973 WATER_PCB-00051303 V "A . State r Iniiana TAT* BOARD OF MKALTH fobrumry M# I860 R@ Eastt Kelly . Mileal Dir*eter Monsanto Chemical Company St Louis 4t Missouri . Dear Booter Kallys ' Thank you very ueh for vw^.jxmgy--lnformatlTo latter of Febru ary 14, relative to tha us a oi^jrocl orslln industry* Iha plant trndor question is the Brasil plant mentionad in your latter* Iha chief oeaplaints ware Irritation of the upper respiratory tract plus possible liver damage* At the time of our study Aroolor was oiroulated in galvanized pipes and most pipes ware 1asking* Xt was suggastad that new pipes be installed and local exhaust ployed* Plant ropiped with copper tubing and inatallad a local azhaust ays tarn ovar axtrudar rolls* Witt this improvaasnt very little Aroelop vapors were escaping* This probably will aolva thair problosi. Further the plant ia considering building an onolosuro around the oxtrudar and roils so that this equipment will ba both anoloaod and exhausted* Thanks again for your help* Voryoruly your*. /kuu ( Ufayto/ VJ IT* Spolyar* M ffl Director Division of Industrial Hygiene Indiana Stata Board of Health WStpn raeas nuun is -rue aw awe ectSMce m momm wium, us *e pcesovica Mvtts&t, * ueaJfit vpi. cimtf ?mdwm eaAs*e geaciittiW srreav.** e.-e. a. 41 EXHIBIT NO.^L. | / T Ul WATER PCB-00051304 it. Loui December 12, 19(6 AROCLOR SWEDEN Mr. D. Wood BRUSSELS A. Arpiao - lltUgSlM (3* R Buchanan - qiqch D.V.N. Hardy - LOUDON R. A. 8t*nrod - RSTBB I do not believe that we can glibly accapt Aroclora aa a synonym for polychlorinatad phanols that were discussed at tha meeting of aclantlata at tha Wannar-tiran Cantra in Stockholm on November 27. Thar* ara polyehlorinatad phanola which presumably could inaluda darlvltlvaa from, or impurities In pantachlorophanol and, aapaoially, 2,4-D and 2,4,5-T. These compounds would ba much more liable to appaar in aalnon, pike* and aaa aaglaa than any derived from Aroclora. There ara many chlorinated polyphenyla that mn bo formed durinc tha manufacture of 2,4,5-T and probably pantachlorophanol, aa vail* Our only problem is whathar or not va want to bring thaaa facta up and have our herbicide program receive another black aye* Thia, X will have to leave to your judgment. I think the question here is primarily an analytical problem. How oan wa find out what product Mr. Jensen is talking about? Can wa compare thaaa chromatographic peaks that Mr. Jensen is describing with anything found in Aroclora, pantachlorophanol, 2,4,3-T, ate? X admit I am out of my depth hare but X think another compound la indicted rather than Aroclor. NEK/1n R. Emmet Kelly, M. D NEV 023924 733979 WATER_PCB-00051305 J X attack* copy M m. latter racaivad isms. Ola tala 1a ftoettolm Z lava sasA aopiaa of tMs latter alaa te tie afpwsp^iat dtpustmati witMa oar iasa Xa ooasidarmtioa of tka laportaaee ipear aaat firm years* ee vold be fxataAsl if je aceld arxmaf fe* Eki* iftteififeiai to be MuiilMtl lef tbe apyropriitJi departments ia ft* keels tmA fcknilx cassMatts tzaeaeittad to ms as sasa m fmmiM.a * feo *.'/*, '' WsMSiM ms iSSM Tme&mmmmeckAMt^Lmmrn --Ji by OTX awwiliaal dtepXt^ttfc eedbalX . . `* * ' * . ^ ralatlee t tbe gfdtle ^oMmm aaationed m Me^rnml' 2 mam4 aatariala* a nU la Ixliumtad to laaxa Is Halo frbhloe is laaaiLed tm laciift* a", tka S.X. aasy oafttiai Isnre bums. Mryiaf . ESfissiaX> la <asresSc? Hittfjjd ia tbe 4z^w bavlaf beam borb*4 late M WATER PCB-00051306 c c : v- r - w ^a m ^ ^ W TM ( RISING &. S X R A M Q OP/BO AKTI Q UAQ mXTQM 34 #1 1 39 44 43 mat 1434. 9#^. SVCAVAM 4f November 28 ,, Monsanto Zurooe muSSLS 3 Belgian Per the attention of Hr. D. WOOD Dear Davids yg; ABCCLOHS As mentioned, there has been sms publicity in Sweden concerning investigations made at the Institution cf Analytical Chemistry at the Stockholm University. These have revealed that a i^cup of products called iUpL--iA* Polychlorinated 31- Phenols f PCS fer short - accumulated- in certain orsanH"o? amaala. They-ays said to b* ; related to DOT and equally poisomous. ; The findings were discussed at a meeting of scientists at the Wermer-Gren Centre in Stockholm on November 22. Below please find a translation of an article in the ; Swedish daily paper "Dagens Nyheter" "It is found in saloon and in pike. It.is found in sea eagle living on fish. It Is found.' on the^sur- face of the needles of the fir treesi that isTSdi the air. It is found is the hair of a-five norths baby... " ' *3 ! . * *..* . The scientists working with biocides have for colons time seen this something as unlacwn "peeks? on /their gas chromatographs and at a meeting-4t the Wtoair Gren Center, Research Assistant Sdrea `Jensen of the Institution for Analytical Chemistry at the Stock holm University could reveal the identity of these peeks. It has been found that they consist of a group of poisons. Polychlorinated BlofaaaaXs. (for snort PCS) which are closely reiaCrT7si equally poisonous as, DOT. FC3 is broken down considerably slower than DOT and gives rise to damagybf liver and sidn. PCS is not SIR 017391 WATER PCB-00051307 rising a iTR*Nj ME5A, Brussels - Mr. 2-. '*( c. used as a herbicide. It is; not; manufaccured in- Sweden but is supposed to- used-, by the Industry' to quite some extent. No special, industry 'cat aa far be accused._of.._bAlns the aca^a^-o^-cscranJ-DAtion.. ' Research Asst. S. Jessea has tested 20Q fishes and. a number of birds. He has takea several samples or air and has reached the conclusion that BC3 Ls equally cornea in, Nature as chlcrinated. hydreearhons.of the type of DDT* DDE, and Lindane. Even fish in Laddjaiaur* in Lapland contain FC3. Mr. Jensen has. also found that ?C3 does not appear in animals living on a vegetarian diet, such as the elk. In the course of his work, Mr. Jensen has not found anything indicating-.that the source of contamina tion cernes frem agricultural additives. It Is, however, obvious already now that K3 is most frequently found in organisms living in water or feeding frem water animals. In all examined pikes PQ was found. Is a sea eagle found dead aicside Stockholm it was found that the liver contained __ .*50.jpg of mercury seg_kl.lo. 76 mg PET and consider ably mora--?C3. The exact figure has sot yet been PC3 is found in water and in air, and not only in' the Swedish air, but also in e.g. London air. to Jeasea has. not yet been in London for sampling but could identify the poison by studying a etaremaro^sm of air published in a British techni cal ^OttnaX. 1 to Jensen har also examined the fair of his family and himself red has found PCS on all samples. Most PC3 was found in. the hair of his wife but most sensational was that the girl aged 5 ssnths had nor* PCB la her hair than her brothers and sisters of 3 Bd 6 years Probably the girl had got the poison via the mother's milk. to the State Jftiaeua to Jensen has examined the . whole collection of sea eagles dating back to lSSO. By testing it could be established that PCS was present only in birds from 194A and thereafter while birds collected before 194* were quite free from PC3 The use of PC3 in Sweden is not established in detail. According to American sources these types of products axe used in the manufacture of a variety of heat- resistant materials. They are used for electrical insulation, for fire-proof heat transport in hydraulic oils, in lubricating oils used at high -j J-Oi STR 017392 WATER PCB-00051308 I s t P C 4 S T P A fM Q M ssels - Mr. "s { w' ;c temperature and pressure* in paint-s; and as- pig ments in various plastics. ?C3 is not- importedonly as such. It is also part of several" finishedproducts. Nothing is known as to the way in whichit reaches the water and the air. According to Mr. Jensen* products containing PCS should, have this openly declared. PCS is equally harmful whether absorbed via. the skin, through the food, or by inhalation. In con tact with the skin it can cause dema. For DDTthe highest permissible concentration in the air has been set at 0.5 - 1 mg/cu.metre. Per PCS it has been mentioned to be 0.5 mg/cu.metre. Mr. Jensen will now try to get more complete analytical material. Ke hopes eventually to be able to disclose the source of the contamination and will also increase his cooperation with tcxccologists and genealogists." Another daily paper, Sveaska Dagbladet, has a similar article. Here it Is mentioned that Mr. Jensen* work ing under Lab orator (Professor) Gunnar Widmark, hasdisclosed facts which will have far-reaching- importance, since the findings have proved a new source of pollu tion of the nature. One of the participants at the meeting was Dr. A.V. Holden of Scotland, scientific contact man between the twelve G.Z.G.D. cambrics, who has established coordinated analysis of chemicals used and found in nature.I I suppose there is no doubt that what has been termed Polychlorinated Biphenyls is equal to Aroclor. There la also no doubt that the published facts will cause considerable unrest in several quarters. We probably will have to have Aroclor registered with the Swedish Board of Poisonous Substances and the industry will have to be particularly careful in handling the'material. The problem in seme eases of course may be the disposal of used material. I understand that there hardly exists a convenient method of destroying Aroclor and that possibly burying umaeable material my be the only answer. We shall be glad to hear from you soon. Yours sincerely. nsNQi STRAMD .1 O i SIR 017393 WATER PCB-00051309 I *4 I I 10 7' ,, 12th January, 1967 Aroolor - Sweden mm/m P.G Benignus, St. Louis G.R. Buchanan, St. Louis BS Cameron, Brussels Br. R Itanet Kelly, St. Loula GR. Graham, New York R.A. Steenrod, St Loula . B, Wood, Brussels J.A. Evans, London R0A0 Baxter, Ruabon 'JAN : 6 1967- On 2nd January 1967 Hr A Richardson of Shell Chemicals1 IHmstall Laboratory, Sittingbourae, Kent talked with me over the telephone concerning the Swedish Press report relating to the identification of "Polyclilorlna-ted Biphenols" os trace contaminant in sea birds, fish etc. Richardson has been working for some years on the similar problem with insecticides such as BBT, which are known to have wide distribution in trace quantities He had already found that the chlorine-oontaining residue contained substances more stable than BBT and Just as StJren Jensen reports he has obtained spectrographic evidence that these are very similar if not identical with Aroclors* He has obtained samples of Aroolors 1242, 1254s 1262 and 54^0 from us,' and would now like to have small samples of any chemically pure Aroolor constituents which we may be able to supply Milligram quantities would suffice for his purpobe Mr Richardson was quite stare that the compounds reported to be "polychlorinated biphenols" are really meant to be polychlorinated biphenyls and as support he has sent me a copy of the synopsis of a paper entitled "Pesticide Analysis1 Presence of Polychlorinated Biphenyls at Residue Malaysia of Biological Sandies" by SBren Jensen and Gunner Widmark (photocopy attached)* . 1 discussed with Richardson the soundness of Jenserfs claims, and was assured that Ms work and findings ax sound Jensen ie on the staff of the. Institute of Analytical Chemistry, University of Stockholm A note on the staff and work of the Institute is attached. Prom this you will aee that Jensen is wholly conoeroed with the analysis of chlorinated pesticides and with the work of stations for routine analysisI I would be glad if to Baxter and to Buchanan would arrange to send me milligram samples of any pure Aroolor constituents that may be available at Ruabon and St Jjouis respectively. WATER PCB-00051310 We recently sent you a translation of a Swedish newspaper article referring to the identification in nature of polychlorinated biphenols. Because some of the uses claimed for the materials fell in line with the uses of our own chlorinated diphenyls, we made a point, during our recent visit,to Sweden, of visiting the research institute involved and discussing their particular programme of work. To e 1 im in at e_ any earlier confusaon that there may have been, I~^hourg~TIki~^o~empHasTse that there -is no j3oub't~tKa""the eHe^TTcaT~which~Ts~Th~ubject~~of~the~ investigation and~the newsrelease, is chXorxnaWct dl~pHSnvrT7iT~Aroclor. '1 The company that supplied the mass spectrometer which was used in the research programme, in fact have recently put out a press release on this work. Although I am horrified by some of the headlines in t^iis press release, it does basically describe the' research programme carried out in Sweden, and describes in clear terms how chlorinated diphenyls were identified. I therefore, enclose a copy for your files. ' Jensens only aim in life as an analytical chemist, was to identify the substances found in his research work on the occurrence of insecticides in nature. The unfortunate'aspect of the situation is the comments which have been added to Jensens work. He showed what was present and unqualified people have made f 1 statements as to the possible effect of what he has found. Summarising the publication position, there were original articles covering the Stockholm conference in the Swedish daily press, and these reports were picked up also by the Danish press. You will have seen from D.V.N. Hardy's memo of the 12th January that it has also been picked up by the Shell Chemicals Laboratory `in Kent, U.K. Jensen also divulged that he had been contacted by the Swedish American press agency who intended to include information about this research work in their monthly review "The Swedish American Journal". There is additionally the press review issued by LKB Productor AB which 1 imagine to have been sent to a numbetechnical journals. M-3. h NEV 022156 ./. .. 732211 WATER PCB-00051311 w G. H. Buchanan St. Louis vj 2 26th January, 1967 Effect in Sweden . , ' This matter was raised with us by every capacitor manufacturer in Sweden that we visited. Fortunately there has not been , too much adverse comment as yet from plant workers since : they have not associated the polychlorinated biphenols mentioned ; in the article with Aroclor or Pyralene used in the Swedish \ factories. Jensen, however, stated that he had been approached : personally by^WeraI~^ori^^lAsjs.o.ciaJfce.d_,.with"'c'h'lorinated diphenyls for non-electrical uses and these workers were__quite . v)orraxr^s to the possible effe^tr^n-th`err~Hialth..* Arrangements are being made in Sweden -for this work to be taken over by one of the medical institutes who hope to study . the toxicology of the poloychlorinated diphenyl residues at the levels of Concentration found by Jensen. Additionally ' a geographical survey is to be carried out to try and determine where the highest concentrations of residue are appearing and, > if possible, to detect from this the method of escape so that more security precautions can be taken. We were asked by Jensen if it was possible for Monsanto to supply any samples of the pure isomers of chlorinated diphenyl since his work indicated at the moment that the lower chlorinated isomers are fairly easily metabolised, and the potentially more dangerous constituents are the more highly chlorinated members. If he can get hold of pure isomers, he would like to carry out some work on comparitive rates of metabolisation. Jensen is forwarding me copies of his mass spectrographs and '' details of sample preparation so that we have all the details : of his research work. The point that I have made to Jensen is the need for`care in any further publication of his work which is made. He accepts that the toxicology of chlorinated diphenyls should only be ` discussed with detailed information about exposure concentrations " and exposure times and that generalised statements out of context can only arouse undue public, concern. If any technical journal takes up the press release from the LKB Productor Company, there is little that Monsanto could, or should do. in the way ' of publishing rebuttals. We do not want, personally as Monsanto ' to get too involved in this question. I am hopeful that we NEV 022i5? / -7009'19 WATER PCB-00051312 | G. R Buchanan : ... st. Louis 3 26th January, 196? ;! ' might persuade Jensen himself to write a letter defining ' the true extent of his own research work and placing his . - , results in their proper perspective It would certainly : be helpful in gaining his further support if we were able : to make available to him any small quantities of pure isomers. i; * ; : Since we are not alone in supplying polychlorinated diphenyls ; to the Scandinavian market# I have drawn this matter to the ! attention of the other askarel manufacturers in Europe. As you will see from the press release one of the major ' points that is made is the difficulty in 'disposing of waste . chlorinated diphenyls and again I must mention that constructive . recommendations of the safe disposal of our materials would .' ' ' be most helpful .. i? fmnmnmm i iit? i '[if!.! | m....... NEV 022158 732213 WATER_PCB-00051313 t Gene V/ilde - General Office# February 13, lW EVIL to,ivm oh CTC^nilVrVfKD BlFEEI'ttLS R, raaot Kelly, M, D. P0 W. V. F, Voycbcf? G. tt, SuclkonEm -----Rcsotuub ~ R. E Kcllof li.-re i & brief imuy of nbai we diBcuroed durinfi our aoettof February 6 in your office# i/e reviewed tto iufontim we tmm received ao Ifar on the oOvcrce publicity to Europe oa j^ychlorimtcd hlpitaaylft* For tl record, we taw received too following iwbLiahed isformtlon. Letter from Danner HMeirk of the Xnetituta ot Analytical Chemistry, University of Otocktoln, fctei December 29# about Ms Mr, Jensen Aftfiniag edue of , too unknown In Mi analyticDl volt m polychlori*te biphenyls, Attached to tola letter waa ft report on the . presence bf polyckloilimted hipheryls at wsidw . analysis of biological. Mlea writ-tea by Mr, Jfimm nd ftmnar Ui&mxk* tewe Wood of cur office sent ue toe UCB prefta twleoae of January ID, 1967, about too QmiiA suocom ia detecting to jolyt^ortetofi bdpbeqyl. A aeno written by Save Wood dated Jtoimty 36 wwirf.irftag lil* iriM.% with Jttwott, Xb* Jto**y 3D, l^T# iftsuo of Owalml TtoeXactsrlxG* yt*c 53. Bate# eanoni about biphenyls to ftmdoA, Thto woo Um first pihUthttA ' iirac^mmipHfcl wn Jj `fchu* tL flL ' Stoator 1% 1366, tt* Wm Boleg&lt Mqtolng, e*TUi4 to article about a now r the wort toot to4 bean dm* by to* Ootwaity of stA .- ' SttCttfetatUy, wSl'af toe*# nvoet* wa4 to* mm t^mm Sue io Hit ^crfcfiBiet of to* Arcelor product* to the (kpil ' Diviftloo* we dotoi4 oa toe ftiHowltm Rlea of ftetion, Sina# oil f to* totloa wptond IMl# tuitola to* *iaiJ of your totoorttar* you ftooepted tot sw$cs^b&llty to follcw threw# a the fotoaoaet NEW 024083 734138 WATER PCB-00051314 2- i propane a etafcaneMi or letter for two by Marketing with cmbomra vim inquire about thio publicity. 2 Yew viH talk to Hen Porrcstal on prcjxiring a pnesw> rdoooo aafl ixilti it until such a tiae that we foel as though it Should be tfdeooed. 3* Oi tone thought to bow wo would eBprootih tod* proHm on & ioxieoloeleal and p'wtmjolastoil t. Stalk to the BCE poqplo after vc defino the perow to oosbust* ' % Ammm for eontiwt with Buyer mod Prodehm* Tw aueatlooft that toopt corals back to our ninde during the neotlng' were that la all of the pTOfpas&oA* publietie^ there hao been nothing bout tl level* that -hewo teen found parUeulariy la the air aaft no one haa defined about what lendL would to caewtdawiA _ ternaML &> Keller brought mt the Met that there roust have ' other products found la this oonplele analysis nd he umaM to JUatereatea 'la knowing what @ttef thieve were f'ouad. . AH of tbeaa ptetioa need fnnndiate attention with the ttaeccyiiott, Of eourse^ of the ^fcherf^ of tbs toxlcoSooSoal and pJmwoolo^aal ^wfnrwwfci^ft-j . Mmm da Hat b tea if ^wr* ta suytMiig Z oaa to oar any way Z eea help la eettlna iha# aetioo* mad getting our together oo that m eea ktt aure our ftrodor buoiioo is not affected ty thie evil j^iblicity. .. . frt u.Var Atf* I/ NEV 024084 734139 WATER PCB-00051315 ho* Monsanto Chemical Company At St. Louis, Mo. June 12, 1956 - Mr. H.X. Nason-M.CL . R.E. Soden-Nltr . L.C. Weger-Nltr ?c Dr. R. Enimr.t Kelly v y.e.iicc-' Dept. Persons 1`resen K. T. Hofmann ` Palm (ph.D.) Scenkaen (Plant Supt., part-time ) Cn the 17th of November, 1953, Baclsche was producing a batch of 1 trich'l orphenol from tetrachiorbenzene when the process exceeded contro pressure and temperatures similar to our incident at Nltro. No one Va injured at the time. Vi thin one weelc, as clean-up was being carried out, the first cases of chlcracnc developed. Fifteen or sixteen cases (6 serious) developed within the next 1-2 months and additional cases showed up during the next 10-12 months until there was a total of 50- 60 cases. 1 did not see our most severe Nltro cases nor have I seen photographs of these cases. The photographs of the worst Badische cases show _ horrible skin eruptions with nearly blister-like welts and seme ulcere lien where infection ensued. Areas involved included the face, neck, arms, ?r.d upper half of the body. It is my impression that their 1 severe cases were much worse than ours. In idlticn to the skin mani festations, their men reported all the additional symptoms as exper iences in our workers, i.e, fatigue, vertigo, loss of libido, painful Joints, etc. About ten days following the incident, and after initial clean-up. Dr. Oettel was asked to expose animals to' the workroom atmosphere. Rat bits (in of>en wire cages) were placed in the operating area for 2^-i;8 hours. There were no obvious symptoms, which developed in the animals until one week after exposure - when they died. Autopsy showed liver : necrosis. Cettel thought there might be virus infection or some othei: cause for death until he exposed additional animals in the department,f others in cages suspended inside the "decontaminated" autoclave, and some in the adjacent department. All died within 1-2 weeks following exposure. Subsequently, animals placed in the cages which had pre viously been in the department died of liver necrosis. A thorough systematic investigation lias isolated impurities in the trichlorphenol process (or residues) which will cause zne same effects in rabbits. Liver necrosis will develop in rabbits at the following doses of the indicated materials: 15-20 mg. of pent&chlor naphthalene 1 mg. of chlorinated diphenyl oxide 0.1 mg. of residue from trichiorphenol disti-iation 0.01 mg. of residue fraction from trichiorphenol (above 230C) *"N "N. Cl 5579 % WATER PCB-00051316 Dr. Oettel believes that the nest potent chloracnogen is a comoour.d sonewhet similar to chlorinated diphenyl oxiae, , but a c i y w 11 j i a b d 11 i a ' r.ded with Don Trl-i o r-'< l jZK .ne noj ecuie s . He : r- reached tr.e came c:: 1 1 e r in at ec -- . r.~ \ "Cj 3, fnri, ; any c r. - or 1 r.a t e. c ;./r. <. acne which has been cue brpr.s cr, .r.atec animal skin tests for . uttering' s work er.d was and {I also learned the production according to Dr they now purchase from Sayei, erial which fails to pass the animal tests ayer that- they have experienced chi oracne during trlchlcrphenol but have now licked the problem'1 Kansen {chemist - Research Director At Elberfeldh' Eadl ache has been able to reproduce Ir. the laboratory the conditions which lead to the incident such as theirs and ours at Nitro and va3 quite surprised that we had not been able to do so. I was not giver, the Nitro process information, i.e., temperatures and pressures, but if I had had this information I am sure that I conic h2*ve obtained Badische's. One of their chemists, a Dr. Palm, sat in ch our dis cussions and was prepared to go into details. Ke did mention that "with 3 mo Is of trichlorpbenol, methyl alcohol, end alkali, and a ter perature of l80C" the process gets out of control. His remarks are in quotes because he does not speak English and I'm not certain of his remarks. . Dr. Oettel would be very happy to receive samples of ar.y of cur materials for Investigation. He would like particularly: i (1) Samples of any of the materials involved in our 19^9 incident Including tetrachlorbenzene, trichiorohenol, or Na salt and any residues from the autoclave or material cleaned from the equipment and structural members. (2) Trichlorphenol (or Na salt) from regular production. (3) Any samples from raw materials,- intermediates, and final product which may have been involved in our cases which developed during our normal 2,A5-T production in the years following the initial incident. CONFIDENTIAL P.1 %sKQl\ WATER PCB-00051317 He would ce happy to exchange freely any and all information with us and Kettering. It was ny suggestion that thl: be direct with Dr. Duskind tc eliminate "third parties.' He w :A routinely send ; and we could request Dr. Su ski n.d C-- likewise. r .hat this night save u .n-u-ss ary 6.i?' i cat Mr. of eff; ;lu.-.bl*' lr f'mat li v;.`. unVers . ana -c expense, > . J*, Ir. VS *. s.cci t. i or. t r.vestiger 1 ,\c on r ^^i'i r i n.vc: 1 m.Jgh t ..-.g h U,Ti cbta 3-T. 2 left with Dr. Oe' cooies of the following: {':) The five (5) reports from tr.e Industrial Hygiene Foundation v.hich discuss their rahoit ear tests. (2) ne^v^er^ng s udc: NJtro, 1953 'Clinical and Environmental Survey at (3) Kettering's report - "Environmental Survey Carried Out In' Building 30, Monsanto Chemical Company at Nitro, February 2, 10$6." Wc reviewed thoroughly Mr. Weger's excellent "History ci'^Chlorac.ne" which he sent to me with covering me no dated May'up, iS5d, and which Included descriptions of Kettering's reports on their human and animal research. I did not give Dr. Cettel a copy of thl3 account becaus., I did not have permission to do so. As a result of my visit, it may be desirable tc edit this report somewhat and add further ' process information before forvjarding this to Badische. Ar.vv Srpe reccnr.enda.tl are implied in the above narrative accouJ of my visit to 3adisehe and must be based on an agreement beat full ar.d complete exchange of information with Badische is desirable and ocssible. EPW;dh Attachment Elmer P. Vfneeler 0>*** X * . ^' \. fS, ' * *v pi *g;Q1 WATER PCB-00051318 This document has been retyped for clarity. From Monsanto Chemical Company Att St. Louis, Mo. Mr. H.K. Nason-M.O. Mr. R.E. Soden-Nitro Mr. L.C. Weger-Nitro Date June 12, 1956 To Dr. R. Emmet Kelly At Medical Dept. Reference subject CHLORACNE CASES AT BADISCHEN ANILIN DUE TO TRICHLORPHENOL Person Present: Dr. H. Oettel Dr. H. T. Hofmann A. Palm (Ph.D.) W. Soenksen (Plant Supt., part-time) . On the 17th of November, 1953, Badische was producing a batch of trichlorphenol from tetrachlorbenzene when the process exceeded control pressure and temperatures similar to our incident at Nitro. No one was injured at the time. Within one week, as clean-up was being carried out, the first cases of chloracne developed. Fifteen or sixteen cases (6 serious) developed within the next 1-2 months and additional cases showed up during the next 10-12 months until there was a total of ' 50-60 cases. I did not see our most severe Nitro cases nor have I seen photographs of these cases. The photographs of the worst Badische cases show horrible skin eruptions with nearly blister-1 i.ke welts and some ulcera( tion where infection ensued. Areas involve included the face, neck, arms, and upper half of the body. It is my impression that their severe cases were much worse than ours. In addition to the skin mani festations, their men reported all the additional symptoms as exper iences in our workers, i.e., fatigue, vertigo, loss of libido, painful joints, etc. About ten days following the incident, and after initial clean-up, Dr. Oettel was asked to expose animals to the workroom atmosphere. Rab bits (in open wire cages) were placed in the operating area for 24-48 hours. There were no obvious symptoms which developed in the animals until one week after exposure - when they died. Autopsy showed liver necrosis. Oettel thought there might be virus infection or some other cause for-death until he exposed additional animals in the department, others in cages suspended inside the "decontaminated" autoclave, and some in the adjacent department. All died within 1-2 weeks following exposure. Subsequently, animals placed in the cages which had pre viously been in the department died of liver necrosis. . A thorough systematic investigation has isolated impurities in the trichlorphenol process (or residues) which will cause the same effects in rabbits. Liver necrosis will develop in rabbits at the following doses of the indicated materials: 15-20 mg. 1 mg. 0.2 mg. 0.01 mg. of pentachlor naphthalene of chlorinated diphenyl oxide of residue from trichlorphenol distillation of residue fraction from trichlorphenol (above 230C) This document has been retxmerl for -?*#-.# WATER PCB-00051319 This document has been retyped for clarity. Dr. Oettel believes that the most potent chloracnogen is a compound somewhat similar to c! 1orinated diphenyl oxide, -------- . /-------but, Cl Cl 0 probably with additional oxygen atoms in the molecules. He has cor responded with Don Irish at Dow who either reached the same conclusion independently or, in mentioning the potential of chlorinateddipheny1 oxide, influenced Oettel's reasoning. Oettel believes, further, that this impurity can show up in the production of any chlorinated phenol allegedly to chlornapthalenes, pentachlorphenol, chlorinated biphenyl, etc. Dr. Oettel has no faith in any animal skin tests for isolating chloracnogens. He was very interested in Kettering's work and was not aware of the publication referred to in Dr. Suskind's first report and which describes the cyclic skin development in new-born rats. (Refer ences Parnell, J.P.s Postnatal Development and Functional Histology of the Sebaceous Glands in the Rat, Am. J. Anat., 85:41, 1949). He is convinced that the Bromsulphalein test reported in the attached reprint is significant. In this regard, Badische routinely uses this test on each batch of trichlorphenol which they now purchase from Bayer, and refuses to accept material which fails to pass the animal tests, (I also learned at Bayer that they have experienced chloracne during the production of trichlorphenol but "have now licked the problem" according to Dr. Hansen (chemist - Research Director At Elberfeld). Badische has been able to reproduce in the laboratory the conditions which lead to the incident such as theirs and ours at Nitro and was quite surprised that we had not been able to do so. I was not given the Nitro process information, i.e., temperatures and pressures, but if I had had this information I am sure that I could have obtained Badische' s. One of their chemists, a Dr. Palm, sat in on our dis cussions and was prepared to go into details. He did mention that "with 3 mols of trichlorphenol, methyl alcohol, and alkali, and a tem perature of 180C" the process gets out of control. His remarks are in quotes because he does not speak English and I'm not certain of his remarks. Dr. Oettel would be very happy to receive samples of any of our materials-for investigation. He would like particularly:1 2 3 (1) Samples of any of the materials involved in our 1949 incident including tetrachlorbenzene, trichlorphenol, or Na salt and any residues from the autoclave or material cleaned from the equipment and structural members. (2) Trichlorphenol (or Na salt) from regular production. (3) Any samples from raw materials, intermediates, and final product which may have been involved in our cases which developed during our normal 2, 4, 5-T production in the years following the initial incident. This document has been retyped for clarity. WATER PCB-00051320 This document has been retyped for clarity. He would be happy to exchange freely any and all nformation with us and Kettering. It was my suggestion that this be direct with Dr. Suskind to eliminate "third parties." He would routinely send carbons of any correspondence to us and we could request Dr. Suskind to do likewise. It is my opinion that this might save unnecessary duplication of effort and expense. In addition, Kettering might obtain valuable information to further their investigation involving human volunteers. I left with Dr. Oettel copies of the following: (1) The five (5) reports from the Industrial Hygiene Foundation which discuss their rabbit ear tests. (2) Kettering * s report - "Clinical and Environmental Survey at Nitro, 1953." (3) Kettering's report - "Environmental Survey Carried Out In Building 30, Monsanto Chemical Company at Nitro, February 2, 1956. " We reviewed thoroughly Mr. Weger's excellent "History of Chloracne" which he sent to me with covering memo dated May 15, 1956, and which included descriptions of Kettering' s reports on their human and animal research. I did not give Dr. Oettel a copy of this account because I did not have permission to do so. As a result of my visit, it may be desirable to edit this report somewhat and add further process information before forwarding this to Badische. Any specific recommendations are implied in the above narrative account of my visit to Badische and must be based on an agreement that full and complete exchange of information with Badische is desirable and possible. EPWsdh Attachment EPW Elmer P. Wheeler This document has been retvoed for olarltv WATER PCB-00051321